CN103962105A - Preparation method of PTES (phenyltriethoxysilane) surface modified bacterial cellulose aerogel oil-absorbing material - Google Patents
Preparation method of PTES (phenyltriethoxysilane) surface modified bacterial cellulose aerogel oil-absorbing material Download PDFInfo
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Abstract
The invention relates to a preparation method of an oil-absorbing material, and aims to provide a preparation method of a PTES (phenyltriethoxysilane) surface modified bacterial cellulose aerogel oil-absorbing material. A novel high-efficiency oil-absorbing material is prepared by modifying the surface of bacterial cellulose aerogel by PTES. The method comprises the following steps: first, cultivation of bacterial cellulose; second, preparation of the bacterial cellulose aerogel; and third, hydrophobic modification of the bacterial cellulose aerogel. According to preparation method, the novel bacterial cellulose aerogel oil-absorbing material is prepared by performing hydrophobic modification on the bacterial cellulose aerogel by PTES; the preparation method is simple and is novel in design; the oil-absorbing material has an environment-friendly effect, is high in biocompatibility, high in absorption efficiency and convenient to salvage, can be recycled repeatedly, and can remove oil thoroughly.
Description
Technical field
The present invention relates to a kind of preparation method of oil absorption material, be specifically related to a kind of PTES(phenyl triethoxysilane) preparation method of surface modification 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 similar leakage of oil event in the world, along with the quickening of industrial society's process, China's oil is polluted day by day severe every year.On May 5th, 2010, U.S.'s Gulf of Mexico crude oil leakage event has caused showing great attention to of international community, 10 left and right blasts on fire in evening April 20 coastal 2010 oil drilling platform local time of southern US Louisiana, cause 7 people's severe injuries, at least 11 people missing, until on July 15th, 2010, British Petroleum Company just announces, new oil-controlling device successfully covers the point of leakage of oil under water, then flows into the Gulf of Mexico without crude oil.The Oil spills event that schedules to last nearly 3 months not only causes huge economic loss, and the pressure bringing to environment is lasting and serious especially, and aquatic ecosystem is caused to serious artificial disturbance.At present the processing method of oil spill accident mainly comprises physics, biological and chemical method, and wherein long efficiency of cutting is low the slower cycle of biological method, and chemical method can produce secondary pollution, and physisorphtion is the method for processing preferably marine oil spill.But the oil absorption material existing on present society has oil suction efficiency low more, oil absorption material itself is also to pollute source, after-treatment inconvenience, high in cost of production shortcoming.Therefore prepare new green environment protection oil absorption material and there is huge economic benefit and environmental benefit.
The compound of cellulose aerogels and cellulose aerogels and other organic sponges can be used to the absorption of marine oil spill, but solo fibre element aeroge intensity is not high, and oil suction efficiency is lower, and number of times capable of circulation is few; Although the compound of cellulose aerogels and organic sponge has improved its intensity, organic sponge itself is scattering in marine site environment is worked the mischief.Bacteria cellulose aeroge oil absorption material has high, natural pollution-free, the advantage such as intensity good, and after-treatment is simple of oil suction efficiency than above these oil absorption materials, 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 bacteria cellulose also has the character of many uniquenesses.Bacteria cellulose without association products such as lignin, pectin and hemicelluloses, has high-crystallinity (can reach 95%, plant cellulose be 65%) and the high degree of polymerization (DP value 2000～8000) compared with plant cellulose; Hyperfine network structure, bacteria cellulose fibre is made up of the fento of the several nanometers of diameter, and than thin many of natural fiber, fento is intertwined to form flourishing hyperfine network structure; The elastic modelling quantity of bacteria cellulose is more than the several times to ten times of general string, and tensile strength is high; Bacterial fibers have very strong moisture holding capacity (water retention values, WRV).The WRV value of the bacteria cellulose of undried is up to more than 1000%, and the moisture holding capacity after freeze drying still exceedes 600%.Swelling ability again through 100 DEG C of dried bacteria celluloses in water is suitable with cotton linter; Bacterial fibers have higher biocompatibility, biodegradability is good; When bacteria cellulose biosynthesis, there is Modulatory character.
Oil suction preferably and post processing, depend primarily on porosity and the pore size of aeroge, also has the hydrophobicity of material.Bacteria cellulose aeroge hole is of moderate size, and porosity is high, but has hydrophily, just can be used as good oil absorption material so need to carry out hydrophobically modified.At present, there is not yet the report of Related Bacteria cellulose aerogels for oil absorption material both at home and abroad.
Summary of the invention
The object of this invention is to provide a kind of preparation method of PTES surface modification bacteria cellulose aeroge oil absorption material, by bacteria cellulose aeroge through PTES(phenyl triethoxysilane) make efficient Novel oil absorption material after surface modification.
The object of the invention is to be achieved through the following technical solutions:
A preparation method for PTES surface modification bacteria cellulose aeroge oil absorption material, concrete operation step is 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 cultivation 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 at 30 ~ 35 DEG C, produces at media surface adularescent or milky superficial layer, is bacteria cellulose film; After preparation finishes, take out bacteria cellulose film, after distilled water repeatedly rinses, immerse in NaOH solution, 80 ± 5 DEG C of heating water bath 80 ~ 140min, remove remaining thalline and culture medium, repeatedly rinse to neutrality by deionized water, dry to constant weight, and obtain 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, CaCO
32 ~ 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, Na
2hPO
40.27 ~ 0.5g, citric acid 0.115 ~ 0.25g, anhydrous MgSO
40.025 ~ 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 bacteria cellulose aquagel according to the mass ratio of 1:30 ~ 50 and deionized water; By the hydrogel obtaining freeze drying 24 ~ 72h in freeze drier, obtain bacteria cellulose aeroge.
Three, the hydrophobically modified of bacteria cellulose aeroge
(1) by iron chloride and PTES(phenyl triethoxysilane) be that 5 ~ 8:1 is dissolved in ethanol according to mass ratio, form evenly orange solution, as applying maceration extract.(2) then bacteria cellulose aeroge is immersed in maceration extract, the complete submergence aeroge of maceration extract, lifts dipping 1 ~ 5h to be less than the speed of 1mm/s.(3) aeroge having flooded is placed in a confined chamber, places one deck pyrroles liquid in the bottom of impregnating gas gel, the distance between impregnating gas gel and pyrroles's liquid is 2 ~ 5 centimetres, under room temperature, places 1 ~ 3h, and volatility pyrroles makes the abundant polymerization of PTES.(4) finally in the baking oven of 90 ~ 100 DEG C, be fully dried 0.5 ~ 2h, obtain the hydrophobicity bacteria cellulose aeroge oil absorption material of black.
The concrete using method of PTES modified bacteria cellulose aeroge oil absorption material prepared by the present invention is as follows: according to the size of oil spill area, the oil absorption material of preparation is cut into 1 × 1cm ~ 50 × 50cm bulk, the block oil absorption material that can be also 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 oil products and the organic solvents such as Russia's oil that the carbon nano-fiber aeroge oil absorption material prepared of the present invention can leak in quick adsorption water in 1 ~ 60min, diesel oil, gasoline, soybean oil, peanut oil, cyclohexane, n-hexane, toluene, absorbency is heavy more than 50 times up to self.After oil suction, can directly salvage with net or other instruments, oil removing is thorough.In addition, the aerogel material after oil suction can be extruded oil by modes such as centrifugal or extruding, and oil absorption material is regenerated, and recycles and still has very high oil suction efficiency for 2 ~ 5 times.
The present invention has following beneficial effect:
1, prepare bacteria cellulose aeroge by BC (bacteria cellulose), bacteria cellulose microfibril diameter is thin, microstructure is regular, and the feature that the bacteria cellulose aeroge of preparation has evenly, porosity is high is advantageous as oil absorption material.The aeroge further obtaining after surface hydrophobicity modification can extensively absorb multiple organic solvent and oil product, and absorbency reaches the more than 50 times of own wt, has good recuperability and selective.
2, the bacteria cellulose aeroge before and after the modification that prepared by the present invention has highly porous three-dimensional net structure, polymerization through PTES on cellulose microfibril and carrying out after hydrophobically modified, aeroge becomes oleophylic, hydrophobicity from original hydrophily, can be for absorbing the organic solvent and the oil product that leak in the water such as ocean.
3, the present invention carries out hydrophobically modified with PTES to bacteria cellulose aeroge and has prepared novel bacteria cellulose aeroge oil absorption material, and preparation method is simple, novel in design, and environment friendly biological compatibility is good, absorption efficiency is high, oil removing is thorough, and it is convenient to salvage, and can repeatedly reuse.
4, the PTES surface modification bacteria cellulose aeroge oil absorption material that prepared by the present invention has good selective oil absorbency, can be advantageously used in water-oil separating or absorb the oil spilling in water, and water body is not polluted, and has a good application prospect.
Detailed description of the invention
Below technical scheme of the present invention is further described, but is not limited to this, every technical solution of the present invention is modified or is equal to replacement, and do not depart from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
Detailed description of the invention one: present embodiment is utilized bacteria cellulose microfibril to dissolve and formed bacteria cellulose aquagel, then bacteria cellulose aeroge is prepared in freeze drying, hydrophobically modified is carried out in bacteria cellulose aeroge surface with PTES, thereby prepare novel, efficient, the environmental protection oil absorption material that can be used for marine oil spill, concrete operation step is as follows:
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, and nitrogenous source is dusty yeast and tryptone; Proportioning is glucose 5g, dusty yeast 1g, agar 2g, CaCO
32g, deionized water 100ml, is adjusted to 6.8 by medium pH.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 agent alcohol, prevent 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, and is inoculated in 100mL fermentation medium 35 DEG C of static cultivation 7d with 10% inoculum concentration.
(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, Na
2hPO
40.27g, citric acid 0.115g, anhydrous MgSO
40.025g, deionized water 100ml, regulates pH to 6.0 ± 0.2, cultivates 7d at 35 DEG C, can see at media surface adularescent or milky superficial layer and producing, and is bacteria cellulose.
(4) after preparation finishes, take out bacteria cellulose film, after distilled water repeatedly rinses, in the NaOH solution that immersion mass concentration is 1%, 80 DEG C of heating water bath 120min, remove remaining thalline and culture medium, repeatedly rinse to neutrality by deionized water, all be 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, the BC after smashing is fully mixedly configured into bacteria cellulose aquagel according to the mass ratio of 1:30 and deionized water.By freezing in refrigerator overnight the hydrogel obtaining, then freeze drying 72h under-48 DEG C, 0.04mbar in freeze drier, obtains bacteria cellulose aeroge.
Three, the hydrophobically modified of bacteria cellulose aeroge
The bacteria cellulose aeroge of preparing in step 2 is carried out respectively in acetone and distilled water to ultrasonic cleaning and remove impurity, fully dry.Iron chloride and PTES(phenyl triethoxysilane) be that 5:1 is dissolved in ethanol according to mass ratio, form an even orange solution, as applying maceration extract.Then dry bacteria cellulose aeroge is later immersed in maceration extract, lift dipping 1h to be less than the speed of 1mm/s.The aeroge having flooded is placed in a confined chamber, places one deck pyrroles liquid in bottom, and the distance between dipping sponge and pyrroles's liquid is 2 centimetres, under room temperature, places 1h, and volatility pyrroles makes the abundant polymerization of PTES.Finally rinse sponge with second alcohol and water and remove unreacted monomer or other byproducts, fully dry 2h in the baking oven of 100 DEG C, the hydrophobicity bacteria cellulose aeroge oil absorption material of acquisition black.
The oil absorption material of preparation is prepared into the oil absorption material of 1 × 1cm size, be placed in the oil spilling of 50 × 50cm area and the mixture of water, add after oil spilling 10g, add the oil absorption material 0.2g of preparation, 5min can oil suction 98%, and Saturation Oil Absorbency reaches 50 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 bacteria cellulose aeroge oil absorption material according to following steps:
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, and nitrogenous source is dusty yeast and tryptone; Proportioning is glucose 5g, dusty yeast 1g, agar 2g, CaCO
32g, deionized water 100ml, is adjusted to 7.0 by medium pH.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 agent alcohol, prevent that acetobacter xylinum is contaminated.
(2) fermented tea adopts bacterium liquid to go down to posterity, and takes out appropriate bacterium liquid from fermented tea liquid (being purchased from Yi Jun family), is inoculated in 100mL fermentation medium 35 DEG C of static cultivation 7d with 20% inoculum concentration.
(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, Na
2hPO
40.27g, citric acid 0.115g, anhydrous MgSO
40.025g, deionized water 100ml, regulates pH to 6.2, cultivates 7d at 35 DEG C, can see at media surface adularescent or milky superficial layer and producing, and is bacteria cellulose.
(4) after preparation finishes, take out bacteria cellulose film, after distilled water repeatedly rinses, in the NaOH solution that immersion mass concentration is 1%, 80 DEG C of heating water bath 120min, remove remaining thalline and culture medium, repeatedly rinse to neutrality by deionized water, all be 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, the BC after smashing is fully mixedly configured into bacteria cellulose aquagel according to the ratio of mass ratio 1:40 and deionized water.By freezing in refrigerator overnight the hydrogel obtaining, then freeze drying 72h under-48 DEG C, 0.04mbar in freeze drier, obtains bacteria cellulose aeroge.
Three, the hydrophobically modified of bacteria cellulose aeroge
The bacteria cellulose aeroge of preparing in step 2 is carried out respectively in acetone and distilled water to ultrasonic cleaning and remove impurity, fully dry.Iron chloride and PTES(phenyl triethoxysilane) be that 7:1 is dissolved in ethanol according to mass ratio, form an even orange solution, as applying maceration extract.Then dry bacteria cellulose aeroge is later immersed in maceration extract, lift dipping 1h to be less than the speed of 1mm/s.The aeroge having flooded is placed in a confined chamber, places one deck pyrroles liquid in bottom, and the distance between dipping sponge and pyrroles's liquid is 4 centimetres, under room temperature, places 1h, and volatility pyrroles makes the abundant polymerization of PTES.Finally rinse sponge with second alcohol and water and remove unreacted monomer or other byproducts, fully dry 2h in the baking oven of 100 DEG C, the hydrophobicity bacteria cellulose aeroge oil absorption material of acquisition black.
The oil absorption material of preparation is prepared into the oil absorption material of 5 × 5cm size, be placed in the oil spilling of 500 × 500cm area and the mixture of water, add after oil spilling 50g, add the oil absorption material 0.8g of preparation, 5min can oil suction 98%, and Saturation Oil Absorbency reaches 62.5 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 PTES surface modification bacteria cellulose aeroge oil absorption material, is characterized in that described method step is as follows:
One, the cultivation of bacteria cellulose;
Two, the preparation of bacteria cellulose aeroge:
The bacteria cellulose that step 1 is cultivated is smashed, and then the bacteria cellulose of smashing and deionized water is fully mixedly configured into bacteria cellulose aquagel; By the hydrogel obtaining freeze drying 24 ~ 72h in freeze drier, obtain bacteria cellulose aeroge;
Three, the hydrophobically modified of bacteria cellulose aeroge
(1) be that 5 ~ 8:1 is dissolved in ethanol by iron chloride and PTES according to mass ratio, form evenly orange solution, as applying maceration extract; (2) then bacteria cellulose aeroge is immersed in maceration extract, lift dipping 1 ~ 5h to be less than the speed of 1mm/s; (3) aeroge having flooded is placed in a confined chamber, places one deck pyrroles liquid in the bottom of impregnating gas gel, under room temperature, place 1 ~ 3h, volatility pyrroles makes the abundant polymerization of PTES; (4) finally in the baking oven of 90 ~ 100 DEG C, be fully dried 0.5 ~ 2h, obtain the hydrophobicity bacteria cellulose aeroge oil absorption material of black.
2. the preparation method of PTES surface modification bacteria cellulose aeroge oil absorption material according to claim 1, it is characterized in that in described step 1, the cultural method of bacteria cellulose is as follows: 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 cultivation 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 at 30 ~ 35 DEG C, produces at media surface adularescent or milky superficial layer, is bacteria cellulose film; After preparation finishes, take out bacteria cellulose film, after distilled water repeatedly rinses, immerse in NaOH solution, 80 ± 5 DEG C of heating water bath 80 ~ 140min, remove remaining thalline and culture medium, repeatedly rinse to neutrality by deionized water, dry to constant weight.
3. the preparation method of PTES surface modification bacteria cellulose aeroge oil absorption material according to claim 2, 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, CaCO
32 ~ 3g, deionized water 100ml, pH=6.8 ~ 7.2.
4. the preparation method of PTES surface modification bacteria cellulose aeroge oil absorption material according to claim 3, 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, CaCO
32g, deionized water 100ml, pH=6.8 ~ 7.2.
5. the preparation method of PTES surface modification bacteria cellulose aeroge oil absorption material according to claim 2, is characterized in that consisting of of described fluid nutrient medium: glucose 2 ~ 3g, dusty yeast 0.5 ~ 1g, tryptone 0.5 ~ 1.5g, Na
2hPO
40.27 ~ 0.5g, citric acid 0.115 ~ 0.25g, anhydrous MgSO
40.025 ~ 0.05g, deionized water 100ml, pH=6.0 ± 0.2.
6. the preparation method of PTES surface modification bacteria cellulose aeroge oil absorption material according to claim 5, is characterized in that consisting of of described fluid nutrient medium: glucose 2g, dusty yeast 0.5g, tryptone 0.5g, Na
2hPO
40.27g, citric acid 0.115g, anhydrous MgSO
40.025g, deionized water 100ml, pH=6.0 ± 0.2.
7. the preparation method of PTES surface modification bacteria cellulose aeroge oil absorption material according to claim 1, is characterized in that in described step 2, and in bacteria cellulose aquagel, the mass ratio of bacteria cellulose and water is 1:30 ~ 50.
8. the preparation method of PTES surface modification bacteria cellulose aeroge oil absorption material according to claim 1, is characterized in that in described step 2, and freeze drying temperature is-48 DEG C, and freeze drying pressure is 0.04mbar.
9. the preparation method of PTES surface modification bacteria cellulose aeroge oil absorption material according to claim 1, is characterized in that in described step 3, and the distance between impregnating gas gel and pyrroles's liquid is 2 ~ 5 centimetres.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105133318A (en) * | 2015-09-25 | 2015-12-09 | 兰州大学 | Silicone-modified mudar floss oil absorption material |
| CN105924686A (en) * | 2016-04-13 | 2016-09-07 | 四川大学 | Biology base polymer aerogel oil absorption material and preparation method thereof |
| CN106675523A (en) * | 2016-12-11 | 2017-05-17 | 汪逸凡 | Preparation method of biodegradable high oil absorption material |
| EP4389802A1 (en) | 2022-12-21 | 2024-06-26 | Bioweg UG | Novel and versatile biodegradable micropowder |
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| JPS63254125A (en) * | 1987-04-09 | 1988-10-20 | Sumitomo Chem Co Ltd | Production of electrically conductive composite material |
| CN103756006A (en) * | 2014-01-20 | 2014-04-30 | 东北林业大学 | Preparation method of ultralight and hydrophobic nano fibrillated cellulose aerogel with high oil absorption |
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2014
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63254125A (en) * | 1987-04-09 | 1988-10-20 | Sumitomo Chem Co Ltd | Production of electrically conductive composite material |
| CN103756006A (en) * | 2014-01-20 | 2014-04-30 | 东北林业大学 | Preparation method of ultralight and hydrophobic nano fibrillated cellulose aerogel with high oil absorption |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105133318A (en) * | 2015-09-25 | 2015-12-09 | 兰州大学 | Silicone-modified mudar floss oil absorption material |
| CN105924686A (en) * | 2016-04-13 | 2016-09-07 | 四川大学 | Biology base polymer aerogel oil absorption material and preparation method thereof |
| CN105924686B (en) * | 2016-04-13 | 2018-10-12 | 四川大学 | A kind of bio-based polymers aeroge oil absorption material and preparation method thereof |
| CN106675523A (en) * | 2016-12-11 | 2017-05-17 | 汪逸凡 | Preparation method of biodegradable high oil absorption material |
| EP4389802A1 (en) | 2022-12-21 | 2024-06-26 | Bioweg UG | Novel and versatile biodegradable micropowder |
| WO2024133650A1 (en) | 2022-12-21 | 2024-06-27 | Bioweg Ug | Novel and versatile biodegradable micropowder |
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