CN104017236B - A kind of preparation method of hybrid inorganic-organic modifying super hydrophobicity bacteria cellulose aeroge oil absorption material - Google Patents
A kind of preparation method of hybrid inorganic-organic modifying super hydrophobicity bacteria cellulose aeroge oil absorption material Download PDFInfo
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Abstract
A preparation method for hybrid inorganic-organic modifying super hydrophobicity bacteria cellulose aeroge oil absorption material, relates to a kind of preparation method of oil absorption material. The preparation method who the object of this invention is to provide a kind of hybrid inorganic-organic modifying super hydrophobicity bacteria cellulose aeroge oil absorption material, bacteria cellulose aeroge obtains hydrophobic aerogels oil absorption material after hybrid inorganic-organic modifying super hydrophobicity. Described method step is as follows: one, the cultivation of bacteria cellulose; Two, the preparation of bacteria cellulose aeroge; Three, the preparation of hybrid inorganic-organic modifying super hydrophobicity bacteria cellulose aeroge. Oil absorption material prepared by the present invention has good selective oil absorbency, can be advantageously used in water-oil separating or absorb the oil spilling leaking in water, water body is not polluted, and be a kind of Novel oil absorption material with very big application potential.
Description
Technical field
The present invention relates to a kind of preparation method of oil absorption material, be specifically related to a kind of hybrid inorganic-organic modifying super hydrophobicityThe preparation method of bacteria cellulose aeroge oil absorption material.
Background technology
In recent years, along with the exploitation day by day of offshore petroleum resources, oil spill accident constantly increases. All can there is every year class in the worldLike leakage of oil event, along with the quickening of industrial society's process, China's oil is polluted day by day severe. On May 5th, 2010, U.S. Mo XiBrother gulf crude oil leakage event has caused showing great attention to of international community, the coastal oil drilling in southern US Louisiana10 left and right blasts on fire in evening April 20 2010 platform local time, cause 7 people's severe injuries, at least 11 people missing, schedule to last nearly 3The Oil spills event of individual month not only causes huge economic loss, and the pressure bringing to environment is lasting and serious, right especiallyAquatic ecosystem causes serious artificial disturbance. The processing method of oil spill accident mainly comprises physics, biological and chemical at presentMethod, wherein biological method is slow, the cycle is long and efficiency is low, and chemical method may produce secondary pollution, physisorphtionIt is the method for processing preferably marine oil spill. But the oil absorption material existing on present society has that oil suction efficiency is low, oil suction material moreMaterial is difficult for degraded, after-treatment inconvenience, high in cost of production shortcoming. Therefore preparing new green environment protection oil absorption material has hugeEconomic benefit and environmental benefit.
The compound of cellulose aerogels and cellulose aerogels and other organic sponges can be used to marine oil spillAbsorption, but solo fibre element aeroge intensity is not high, oil suction efficiency is lower, and number of times capable of circulation is few; Cellulose airsettingAlthough the compound of glue and organic sponge has improved its intensity, organic sponge itself is scattering in marine site environment is caused to dangerEvil. It is high, natural pollution-free, strong that bacteria cellulose aeroge oil absorption material has oil suction efficiency than above these oil absorption materialsSpend, the advantage such as after-treatment is simple, is the aeroge oil absorption material that a kind of future development has application potential very much.
The native cellulose that bacteria cellulose and plant or marine alga produce all has identical molecular structure unit, but bacteriumCellulose also has the character of many uniquenesses. Bacteria cellulose compared with plant cellulose without lignin, pectin and hemicelluloseDeng association product, have high-crystallinity (can reach 95%, plant cellulose be 65%) and the high degree of polymerization (DP value 2000～8000); Hyperfine network structure, bacteria cellulose fibre is made up of the fento of the several nanometers of diameter, thinner than natural fiberMany, fento is intertwined to form flourishing hyperfine network structure; The elastic modelling quantity of bacteria cellulose is general stringMore than several times to ten times, and tensile strength is high; Bacterial fibers have very strong moisture holding capacity (waterretentionValues, WRV). The WRV value of the bacteria cellulose of undried is up to more than 1000%, and the moisture holding capacity after freeze drying is still superCross 600%. Swelling ability again through 100 DEG C of dried bacteria celluloses in water is suitable with cotton linter; Bacterial fibers haveHigh biocompatibility, biodegradability are good; When bacteria cellulose biosynthesis, there is Modulatory character.
Oil suction preferably and post processing, depend primarily on aeroge porosity, pore size and material dredgeWater, lipophilicity. Bacteria cellulose aeroge hole is of moderate size, and porosity is high, after distinct methods is processed, can haveHigh hydrophobicity is good oil absorption material. At present, there is not yet Related Bacteria cellulose aerogels both at home and abroad for oil suction materialThe report of material.
Summary of the invention
The object of this invention is to provide a kind of hybrid inorganic-organic modifying super hydrophobicity bacteria cellulose aeroge oil absorption materialPreparation method, bacteria cellulose aeroge obtains hydrophobic aerogels oil suction after hybrid inorganic-organic modifying super hydrophobicityMaterial.
The object of the invention is to be achieved through the following technical solutions:
A preparation method for hybrid inorganic-organic modifying super hydrophobicity bacteria cellulose aeroge oil absorption material, specifically behaviourMake step as follows:
One, the cultivation of bacteria cellulose
Fermented tea liquid is inoculated into 100mL with 10 ~ 20% inoculum concentration and goes down to posterity in culture medium, 30 ~ 35 DEG C of static cultivations 5 ~7d; Then the bacterial plaque that picking is transparent from the culture medium that goes down to posterity is transferred in fluid nutrient medium, cultivates 5 ~ 7d, in training at 30 ~ 35 DEG CSupport primary surface adularescent or milky superficial layer and produce, be bacteria cellulose film; After preparation finishes, take out bacteria celluloseFilm, after distilled water repeatedly rinses, immerses in NaOH solution, 80 ± 5 DEG C of heating water bath 80 ~ 140min, remove remaining thalline andCulture medium, rinses to neutrality repeatedly by deionized water, dries to constant weight, and obtains BC film.
In above-mentioned steps, described in go down to posterity the consisting of of culture medium: glucose 5 ~ 7g, dusty yeast 1 ~ 2g, agar 2 ~ 5g,CaCO32 ~ 3g, deionized water 100ml, pH=6.8 ~ 7.2.
In above-mentioned steps, the consisting of of described fluid nutrient medium: glucose 2 ~ 3g, dusty yeast 0.5 ~ 1g, tryptone 0.5~1.5g，Na2HPO40.27 ~ 0.5g, citric acid 0.115 ~ 0.25g, anhydrous MgSO40.025 ~ 0.05g, deionized water 100ml, pH=6.0±0.2。
Two, the preparation of bacteria cellulose aeroge
BC film is smashed, the BC after smashing is fully mixedly configured into according to the mass ratio of 1:30 ~ 50 and deionized waterBacteria cellulose aquagel; By the hydrogel obtaining freeze drying 24 ~ 72h in freeze drier, obtain bacteria cellulose gasGel.
Three, the preparation of hybrid inorganic-organic modifying super hydrophobicity bacteria cellulose aeroge
(1) in there-necked flask, add successively organosilicon acrylic resin, MTES(methyl according to the ratio of 5 ~ 8:1 ~ 3:1 ~ 3:12 ~ 20Triethoxysilane), TEOS(ethyl orthosilicate) and ethanol, stir at normal temperatures 1 ~ 2h;
(2) the bacteria cellulose aeroge preparing is added in above-mentioned mixing material, stir lower dipping 2 ~ 10h, controlAeroge and above-mentioned mixing material mass ratio are 10 ~ 15:1;
(3) adding mass concentration is 5 ~ 7% ammoniacal liquor, and the addition of ammoniacal liquor is 10 ~ 20% of mixed liquor quality, continues to stir2 ~ 5h, takes out afterwards room temperature and dries, and dries 1 ~ 3h at 100 ~ 120 DEG C, can obtain the bacterial fibers of hybrid inorganic-organic modificationElement aeroge oil absorption material.
Hybrid inorganic-organic modified bacteria cellulose aeroge oil absorption material prepared by the present invention carries out system testing,The concrete using method of oil absorption material is as follows: according to the size of oil spill area, preparation oil absorption material be cut into 1 × 1cm ~ 50 ×50cm bulk, can be also that the block oil absorption material of sizes mixes use, has ensured quick, the completeness of oil suction.
Carry out the absorption test of oil spilling in water by this using method, find carbon nano-fiber aeroge suction prepared by the present inventionOil products such as Russia's oil that light wood material can leak in quick adsorption water in 15min, diesel oil, gasoline, cyclohexane, toluene and havingMachine solvent, absorbency is heavy 50 ~ 70 times up to self. After oil suction, can directly salvage with net or other utensils oil removal rateHigher. In addition, the aerogel material after oil suction can be extruded oil by modes such as centrifugal or extruding, and oil absorption material is able to againRaw, recycle and still there is very high oil suction efficiency for several times.
The present invention has following beneficial effect:
1, bacteria cellulose microfibril diameter is thin, microstructure is regular, the bacteria cellulose aeroge loose structure of preparationFully, the hybrid inorganic-organic modifying super hydrophobicity bacteria cellulose aeroge oil absorption material of preparing through surface modification treatment is usedWhile making adsorbent, can extensively absorb multiple organic solvent, oil product etc., there is good recuperability and selective.
2, the existence of the little mastoid process of the micron order of rough surface and surperficial wax makes it have super-hydrophobic, oleophylic performance, inhalesReceipts ability can reach 50 ~ 70 times to own wt.
3, the hybrid inorganic-organic modified bacteria cellulose aeroge oil absorption material that prepared by the present invention has the three-dimensional of porousNetwork structure.
Hybrid inorganic-organic modified bacteria cellulose aeroge oil absorption material preparation method that 4, prepared by the present invention is simple,Cost is low, and environment friendly biological compatibility is good, pollution-free, and oil suction efficiency is high, can repeatedly reuse.
5, the oil absorption material that prepared by the present invention has good selective oil absorbency, can be advantageously used in water-oil separatingOr the oil spilling leaking in absorption water, water body is not polluted, be a kind of Novel oil absorption material with very big application potential.
Detailed description of the invention
Below technical scheme of the present invention is further described, but is not limited to this, every to the technology of the present inventionScheme is modified or is equal to replacement, and does not depart from the spirit and scope of technical solution of the present invention, all should be encompassed in the present inventionProtection domain in.
Detailed description of the invention one: present embodiment is utilized bacteria cellulose microfibril to dissolve and formed bacteria cellulose water-settingGlue, then bacteria cellulose aeroge is prepared in freeze drying, and then organic and inorganic is carried out in bacteria cellulose aeroge surface and mixChange modifying super hydrophobicity, make the oil absorption material that can be used as marine oil spill, concrete operation step is as follows:
The cultivation of step 1, bacteria cellulose
(1) the fermented tea liquid culture medium that goes down to posterity: culture medium is made up of agar, and carbon source is glucose, nitrogenous source be dusty yeast withTryptone; Proportioning is glucose 5g, dusty yeast 1g, agar 2g, CaCO32g, deionized water 100ml, is more than best proportioningBut also fine-tuning, medium pH is adjusted to 6.8. Large mouthful vial is cleaned to twice with alcohol, then boil two points with boiling waterClock, removes miscellaneous bacteria and cleaning agent alcohol as far as possible, prevents that acetobacter xylinum is contaminated.
(2) fermented tea adopts bacterium liquid to go down to posterity, and takes out appropriate bacterium liquid from the fermented tea liquid (being purchased from Yi Jun family) of buying, with10% inoculum concentration is inoculated in 100mL fermentation medium, 35 DEG C of static cultivation 7d.
(3) bacterial plaque that picking is transparent from the culture medium that goes down to posterity is transferred in fluid nutrient medium. Consisting of of fluid nutrient medium:Glucose 2g, dusty yeast 0.5g, tryptone 0.5g, Na2HPO40.27g, citric acid 0.115g, anhydrous MgSO40.025g, goesIonized water 100ml, regulates pH to 6.0 ± 0.2, cultivates 7d at 35 DEG C, can see in media surface adularescent or milkySuperficial layer produce, be bacteria cellulose.
(4) after preparation finishes, take out bacteria cellulose film, after distilled water repeatedly rinses, immerse 1%(mass concentration)In NaOH solution, 80 DEG C of heating water bath 120min, remove remaining thalline and culture medium, repeatedly rinse to neutrality by deionized waterAfter, be all transferred in glass sand hourglass, dry to constant weight at 105 DEG C, obtain BC film.
The preparation of step 2, bacteria cellulose aeroge
The rectangle that BC film is cut into small pieces or cubic shape, and smash, by the BC after smashing according to the mass ratio of 1:30 withDeionized water is fully mixedly configured into bacteria cellulose aquagel. By freezing in refrigerator overnight the hydrogel obtaining, then inIn freeze drier, freeze drying 72h under-48 DEG C, 0.04mbar, obtains bacteria cellulose aeroge; Be ground into block for subsequent use.
The preparation of step 3, hybrid inorganic-organic modifying super hydrophobicity bacteria cellulose aeroge
(1) ratio that is 5:1:1:12 according to mass ratio in there-necked flask adds organosilicon acrylic resin, MTES(methyl three successivelyEthoxysilane), TEOS(ethyl orthosilicate) and ethanol,, stir at normal temperatures 1h;
(2) the bacteria cellulose aeroge preparing is added in above-mentioned mixing material, stir lower dipping 5h, control airsettingGlue and above-mentioned mixing material mass ratio are 10:1;
(3) adding mass concentration is 5% ammoniacal liquor, and the addition of ammoniacal liquor is 10% of mixed liquor quality, continues to stir 5h, itRear taking-up room temperature is dried, and dries 3h at 100 DEG C, can obtain the bacteria cellulose aeroge oil suction of hybrid inorganic-organic modificationMaterial.
The oil absorption material of preparation is prepared into the oil absorption material of 1 × 1cm size, is placed in oil spilling and the water of 50 × 50cm areaMixture in, add after oil spilling 10g, add the oil absorption material 0.1g of preparation, 5min can oil suction 98%, Saturation Oil Absorbency reachesTo 100 times of own wt. Employing is dragged for oil network and is salvaged, and oil suction is thorough, protects oily rate high, reaches 99%.
Detailed description of the invention two: present embodiment is prepared the bacterial fibers of hybrid inorganic-organic modification according to following stepsElement aeroge oil absorption material:
One, the cultivation of bacteria cellulose
(1) the fermented tea liquid culture medium that goes down to posterity: culture medium is made up of agar, and carbon source is glucose, nitrogenous source be dusty yeast withTryptone; Proportioning is glucose 5g, dusty yeast 1g, agar 2g, CaCO32g, deionized water 100ml, regulates medium pHTo 7.0. Large mouthful vial is cleaned to twice with alcohol, then boil two minutes with boiling water, remove as far as possible miscellaneous bacteria and cleaning agentAlcohol, prevents that acetobacter xylinum is contaminated.
(2) fermented tea adopts bacterium liquid to go down to posterity, and from fermented tea liquid (being purchased from Yi Jun family) the appropriate bacterium liquid of taking-up, with 20%Inoculum concentration is inoculated in 100mL fermentation medium, 35 DEG C of static cultivation 7d.
(3) bacterial plaque that picking is transparent from the culture medium that goes down to posterity is transferred in fluid nutrient medium. Consisting of of fluid nutrient medium:Glucose 2g, dusty yeast 0.5g, tryptone 0.5g, Na2HPO40.27g, citric acid 0.115g, anhydrous MgSO40.025g, goesIonized water 100ml, regulates pH to 6.2, cultivates 7d at 35 DEG C, can see on media surface adularescent or milky surfaceLayer produces, and is bacteria cellulose.
(4) after preparation finishes, take out bacteria cellulose film, after distilled water repeatedly rinses, immersion mass concentration is 1%In NaOH solution, 80 DEG C of heating water bath 120min, remove remaining thalline and culture medium, repeatedly rinse to neutrality by deionized waterAfter, be all transferred in glass sand hourglass, dry to constant weight at 105 DEG C, obtain BC film.
Two, the preparation of bacteria cellulose aeroge
The rectangle that BC film is cut into small pieces or cubic shape, and smash, by the BC after smashing according to the ratio of mass ratio 1:40Example is fully mixedly configured into bacteria cellulose aquagel with deionized water. By freezing in refrigerator overnight the hydrogel obtaining, soAfter in freeze drier freeze drying 72h under-48 DEG C, 0.04mbar, obtain bacteria cellulose aeroge.
Three, the preparation of hybrid inorganic-organic modifying super hydrophobicity bacteria cellulose aeroge
(1) ratio that is 5:1:1:12 according to mass ratio in there-necked flask adds organosilicon acrylic resin, MTES(methyl three successivelyEthoxysilane), TEOS(ethyl orthosilicate) and ethanol,, stir at normal temperatures 1h;
(2) the bacteria cellulose aeroge preparing is added in above-mentioned mixing material, stir lower dipping 5h, control airsettingGlue and above-mentioned mixing material mass ratio are 10:1;
(3) adding mass concentration is 5% ammoniacal liquor, and the addition of ammoniacal liquor is 10% of mixed liquor quality, continues to stir 3h, itRear taking-up room temperature is dried, and dries 3h at 100 DEG C, can obtain the bacteria cellulose aeroge oil suction of hybrid inorganic-organic modificationMaterial.
The oil absorption material of preparation is prepared into the oil absorption material of 1 × 1cm size, is placed in oil spilling and the water of 50 × 50cm areaMixture in, add after oil spilling 10g, add the oil absorption material 0.17g of preparation, 5min can oil suction 98%, Saturation Oil Absorbency reachesTo 80 times of own wt. Employing is dragged for oil network and is salvaged, and oil suction is thorough, protects oily rate high, reaches 99%.
Claims (9)
1. a preparation method for hybrid inorganic-organic modifying super hydrophobicity bacteria cellulose aeroge oil absorption material, its feature existsAs follows in described method step:
One, the cultivation of bacteria cellulose;
Two, the preparation of bacteria cellulose aeroge:
The bacteria cellulose that step 1 is cultivated is smashed, then by the bacteria cellulose of smashing and the abundant mixed configuration of deionized waterBecome bacteria cellulose aquagel; By the hydrogel obtaining freeze drying 24 ~ 72h in freeze drier, obtain bacteria celluloseAeroge;
Three, the preparation of hybrid inorganic-organic modifying super hydrophobicity bacteria cellulose aeroge:
(1) in there-necked flask according to the mass ratio of 5 ~ 8:1 ~ 3:1 ~ 3:12 ~ 20 add successively organosilicon acrylic resin, MTES, TEOS andEthanol, stirs 1 ~ 2h at normal temperatures;
(2) the bacteria cellulose aeroge preparing is added in above-mentioned mixing material, stir lower dipping 2 ~ 10h;
(3) add ammoniacal liquor, the addition of ammoniacal liquor is 10 ~ 20% of mixed liquor quality, continues to stir 2 ~ 5h, takes out afterwards room temperature and dries in the airDry, dry 1 ~ 3h at 100 ~ 120 DEG C, can obtain the bacteria cellulose aeroge oil absorption material of hybrid inorganic-organic modification.
2. the system of hybrid inorganic-organic modifying super hydrophobicity bacteria cellulose aeroge oil absorption material according to claim 1Preparation Method, is characterized in that, in described step 1, the cultural method of bacteria cellulose is as follows: by fermented tea liquid with 10 ~ 20% connectThe amount of kind is inoculated into 100mL and goes down to posterity in culture medium, 30 ~ 35 DEG C of static cultivation 5 ~ 7d; Then from the culture medium that goes down to posterity, picking is transparentBacterial plaque is transferred in fluid nutrient medium, cultivates 5 ~ 7d at 30 ~ 35 DEG C, produces at media surface adularescent or milky superficial layerRaw, be bacteria cellulose film; After preparation finishes, take out bacteria cellulose film, after distilled water repeatedly rinses, immerse NaOH solutionIn, 80 ± 5 DEG C of heating water bath 80 ~ 140min, remove remaining thalline and culture medium, repeatedly rinse to neutrality by deionized waterAfter, dry to constant weight.
3. the system of hybrid inorganic-organic modifying super hydrophobicity bacteria cellulose aeroge oil absorption material according to claim 2Preparation Method, the consisting of of the culture medium that goes down to posterity described in it is characterized in that: glucose 5 ~ 7g, dusty yeast 1 ~ 2g, agar 2 ~ 5g, CaCO32~ 3g, deionized water 100ml, pH=6.8 ~ 7.2.
4. the system of hybrid inorganic-organic modifying super hydrophobicity bacteria cellulose aeroge oil absorption material according to claim 3Preparation Method, the consisting of of the culture medium that goes down to posterity described in it is characterized in that: glucose 5g, dusty yeast 1g, agar 2g, CaCO32g, go fromSub-water 100ml, pH=6.8 ~ 7.2.
5. the system of hybrid inorganic-organic modifying super hydrophobicity bacteria cellulose aeroge oil absorption material according to claim 2Preparation Method, is characterized in that consisting of of described fluid nutrient medium: glucose 2 ~ 3g, and dusty yeast 0.5 ~ 1g, tryptone 0.5 ~1.5g，Na2HPO40.27 ~ 0.5g, citric acid 0.115 ~ 0.25g, anhydrous MgSO40.025 ~ 0.05g, deionized water 100ml, pH=6.0±0.2。
6. the system of hybrid inorganic-organic modifying super hydrophobicity bacteria cellulose aeroge oil absorption material according to claim 5Preparation Method, is characterized in that consisting of of described fluid nutrient medium: glucose 2g, and dusty yeast 0.5g, tryptone 0.5g,Na2HPO40.27g, citric acid 0.115g, anhydrous MgSO40.025g, deionized water 100ml, pH=6.0 ± 0.2.
7. the system of hybrid inorganic-organic modifying super hydrophobicity bacteria cellulose aeroge oil absorption material according to claim 1Preparation Method, is characterized in that in described step 2, in bacteria cellulose aquagel the mass ratio of bacteria cellulose and water be 1:30 ~50。
8. the system of hybrid inorganic-organic modifying super hydrophobicity bacteria cellulose aeroge oil absorption material according to claim 1Preparation Method, is characterized in that in described step 2, freeze drying temperature is-48 DEG C, and freeze drying pressure is 0.04mbar.
9. the system of hybrid inorganic-organic modifying super hydrophobicity bacteria cellulose aeroge oil absorption material according to claim 1Preparation Method, is characterized in that in described step 3, aeroge and mixing material mass ratio are 10 ~ 15:1.
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| CN106675523A (en) * | 2016-12-11 | 2017-05-17 | 汪逸凡 | Preparation method of biodegradable high oil absorption material |
| CN107513177B (en) * | 2017-09-30 | 2020-09-04 | 中国林业科学研究院林产化学工业研究所 | Vegetable oil modified bacterial cellulose aerogel oil absorption material and preparation method thereof |
| CN108031447B (en) * | 2017-12-25 | 2020-06-19 | 吉林大学 | Cellulose/silicon oxide composite aerogel elastomer, preparation method and application thereof in oil-water separation field |
| CN108031448A (en) * | 2017-12-27 | 2018-05-15 | 西北师范大学 | A kind of preparation method of zein base porous hydrophobic oil absorption material |
| CN108794799A (en) * | 2018-07-06 | 2018-11-13 | 佛山市陵谐环保科技有限公司 | A kind of preparation method of porous absorption oil absorption material |
| CN111097388A (en) * | 2018-10-26 | 2020-05-05 | 南京化学工业园环保产业协同创新有限公司 | Preparation of biodegradable oil absorption material |
| CN110982114B (en) * | 2019-12-11 | 2022-05-27 | 中国科学院苏州纳米技术与纳米仿生研究所 | Aramid fiber/carbon nanotube hybrid aerogel film, and preparation method and application thereof |
| CN111470486B (en) * | 2020-04-14 | 2022-01-25 | 陕西煤业化工技术研究院有限责任公司 | Three-dimensional silicon-carbon composite negative electrode material, preparation method thereof and application thereof in lithium ion battery |
| CN114985431B (en) * | 2022-05-12 | 2023-04-18 | 南华大学 | Modified fiber composite material based on microorganism reinforcement process and preparation method thereof |
| CN114752083A (en) * | 2022-05-26 | 2022-07-15 | 华中科技大学 | Method for in-situ culture of bacterial cellulose hydrogel microspheres by using super-hydrophobic interface |
| CN115960384B (en) * | 2023-01-10 | 2024-03-08 | 福州大学 | Elastic bacterial cellulose composite aerogel with structure regulated by absolute ethyl alcohol, and preparation method and application thereof |
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