CN103806130A - Preparation method for bacterial cellulose-based nano active carbon fibers - Google Patents
Preparation method for bacterial cellulose-based nano active carbon fibers Download PDFInfo
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- CN103806130A CN103806130A CN201410063237.4A CN201410063237A CN103806130A CN 103806130 A CN103806130 A CN 103806130A CN 201410063237 A CN201410063237 A CN 201410063237A CN 103806130 A CN103806130 A CN 103806130A
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Abstract
The invention discloses a preparation method for bacterial cellulose-based nano active carbon fibers, and relates to a preparation technology of active carbon materials. The preparation method comprises the following steps: carrying out purification treatment on bacterial cellulose obtained by bacterial fermentation, freezing and drying; then putting the dried bacterial cellulose material into an atmosphere furnace to be subjected to carbonization treatment and heating to 550-600 DEG C; after cooling the material, putting the material into a potassium hydroxide water solution to be immersed for 10-30 minutes; drying and carrying out further activation treatment; and cooling to obtain a bacterial cellulose-based nano active carbon fiber material with a three-dimensional network structure. The preparation process is simple and feasible, is convenient to operate and is low in cost; the obtained bacterial cellulose-based nano active carbon fibers have a good space network structure, high specific surface area, and very good adsorption capacity and adsorption speed; the bacterial cellulose-based nano active carbon fibers are conveniently desorbed and can be applied to the fields of biomedical application, environment protection, wastewater and waste gas treatment and the like.
Description
Technical field
The present invention relates to active carbon material field, refers to especially a kind of preparation method of bacteria cellulose base nanometer activated carbon fiber.
Background technology
Activated carbon is a kind of porous carbon through activation processing, has extremely strong adsorption capacity, the existing century-old history of application in fields such as military affairs, chemical industry, environmental protection.Activated carbon fiber is the third generation activated carbon products after powdered activated carbon and grain active carbon, is a class porous fiber shape sorbing material.It has bigger serface, loose structure and strong surface reaction, and its special fibrous physics form makes itself and adsorbate have larger contact area, thereby has the absorption property of wide spectrum and high adsorption capacity.Compared with powdery, granule activated carbon, the micro mist dirt that activated carbon fiber in use produces is few, can make as required the various products such as felt, cloth, paper, more flexible when use.Therefore, activated carbon fiber more and more receives people's concern in the application of the aspects such as chemical industry, environmental protection, electronics industry, medical, food hygiene.
Carbon nano-fiber refers to the activated carbon fiber with nanoscale, in many performance basis of activated carbon fiber, increase nano effect, make nanometer activated carbon fiber there is stronger adsorption capacity, adsorption rate faster, can meet the instructions for use of the field nano-devices such as military affairs, environmental protection, biology, medical treatment or the multipair active-carbon fibre material of Ultraprecision Equipment simultaneously.
Bacteria cellulose is a kind of natural biopolymer, has hyperfine network structure, is combined into the thick fibre bundle of 40～60 nanometers by the fento of diameter 3～4 nanometers, and is intertwined to form flourishing hyperfine network structure.The characteristic of high-purity, high-crystallinity, high polymerization degree and the numberator height orientation of bacteria cellulose, makes it have the primary condition that becomes nanometer activated carbon fiber presoma.
This patent adopts the presoma as nanometer activated carbon fiber through the bacteria cellulose of special treatment, and through carbonization treatment, activation processing, finally obtains having the nanometer activated carbon fiber material of three-dimensional net structure.Preparation is simple in the present invention, easy to operate, cost is low; the bacteria cellulose base nanometer activated carbon fiber obtaining has good spacial framework, high-specific surface area, splendid adsorption capacity and the rate of adsorption, can be applicable to the fields such as bio-medical, environmental protection, electronic apparatus.
Summary of the invention
The object of this invention is to provide a kind of preparation method of bacteria cellulose base nanometer activated carbon fiber.Relate to a kind of active carbon material technology of preparing.Preparation is simple in the present invention, easy to operate, cost is low; the bacteria cellulose base nanometer activated carbon fiber obtaining has good spacial framework, high-specific surface area, even aperture distribution, splendid adsorption capacity and the rate of adsorption, can be applicable to the fields such as bio-medical, environmental protection, wastewater and waste gas treatment.
The preparation method who discloses a kind of bacteria cellulose base nanometer activated carbon fiber of the present invention, comprise: by the bacteria cellulose purification process, the freeze drying that are obtained by bacterial fermentation, then dried bacteria cellulose material is put into atmosphere furnace carbonization treatment and be heated to 550 ℃～600 ℃, the potassium hydroxide aqueous solution of putting into 10～30wt% after material cooled soaks 10～30min, after oven dry, through further activation processing, obtain having the bacteria cellulose base nanometer activated carbon fiber material of three-dimensional net structure after cooling.
As preferred technical scheme:
Wherein, the preparation method of a kind of bacteria cellulose base nanometer activated carbon fiber as above, described bacterium refers to and can, by the bacterial strain of fermented-producing bacteria cellulose, comprise: one or more in acetobacter xylinum, rhizobium, Sarcina, pseudomonas, achromobacter, Alcaligenes, Aerobacter or azotobacter.
The preparation method of a kind of bacteria cellulose base nanometer activated carbon fiber as above, described purification process refers to, bacteria cellulose is through sodium hydrate aqueous solution thermophilic digestion 10～30min of 10～20wt%.In the bacteria cellulose raw material of bacterial fermentation, have the residual body of a large amount of bacteriums, these residues form local defect by material in the process of carbonization, activation, have a strong impact on porous aperture and the three-dimensional net structure of the nanometer activated carbon fiber obtaining.Sodium hydroxide solution boiling can thoroughly be removed mycoprotein and be sticked to the residual media on cellulose membrane, guarantees the cellulose high-purity of bacteria cellulose material.Meanwhile, NaOH can play certain activation in follow-up activation processing.
The preparation method of a kind of bacteria cellulose base nanometer activated carbon fiber as above, described freeze drying refers to the bacteria cellulose after purification process freezing 12～24h, then vacuumize 24～48h at-20 ℃～-80 ℃.Three-dimensional network microstructure when freeze drying object is to maintain bacteria cellulose hygrometric state.
The preparation method of a kind of bacteria cellulose base nanometer activated carbon fiber as above; described carbonization treatment refers to that bacteria cellulose material is under vacuum, argon gas or nitrogen protection; be warming up to 550 ℃～600 ℃ by room temperature; wherein 100～300 ℃ of interval heating rates are 5～10 ℃/min; 300～500 ℃ of interval heating rates are 1～5 ℃/min, and 500～600 ℃ of interval heating rates are 30 ℃/min.In this patent, calefactive interzone is divided into three sections of controls, 100～300 ℃ of intervals are mainly bacteria cellulose and lose physical absorption water, Hydrogenbond water and intermolecular hydrogen bonding, intramolecular hydrogen bond fracture decomposition; 300～500 ℃ of intervals are mainly the fracture of bacteria cellulose carbochain decomposes, and generates a small amount of volatilization gas.These two keys that calefactive interzone is material carbonisation, in bacteria cellulose carbonisation, quality can significantly reduce, and volume can be along with contraction.In the meantime in order to maintain the original three-dimensional net structure of bacteria cellulose, must the strict heating rate of controlling carbonisation, prevent that the too fast network structure that causes of heating rate from subsiding.
The preparation method of a kind of bacteria cellulose base nanometer activated carbon fiber as above; described activation processing refer to potassium hydroxide aqueous solution soak after material put into nitrogen protection activation furnace heat up heating; heating-up temperature is 700～900 ℃, and temperature retention time is 10～60min.The carbon fiber soaking with potassium hydroxide aqueous solution, in heating process along with the evaporation of fibrous inside steam, can go out the potassium hydroxide granule that some are evenly distributed in fiber surface crystallization, in the time that activating treatment temperature raises, these granule original positions are reacted with carbon, etch some at the equally distributed nanometer micropore of fiber surface, as the interface of continuing reaction, along with the continuation of activation temperature raises, the steam of part metals potassium, sylvite is got between carbon-coating, and the activation of whole carbon fiber is played to facilitation.In like manner, in bacteria cellulose purification process process, residual NaOH also has the active effect that potassium hydroxide is identical.Therefore, in the present invention, the activation effect of activated carbon fiber is the synergistic result of NaOH and potassium hydroxide.
The preparation method of a kind of bacteria cellulose base nanometer activated carbon fiber as above, described coolingly refers to that the bacteria cellulose material heating up after finishing slowly cools to room temperature in atmosphere furnace or activation furnace.
The preparation method of a kind of bacteria cellulose base nanometer activated carbon fiber as above, described bacteria cellulose base nanometer activated carbon fiber material refers to that activated carbon fiber diameter is about 10～30nm, is evenly distributed with 0.5～2nm micropore and has three-dimensional network space structure on fiber.
Compared with prior art, the invention has the beneficial effects as follows:
The present invention adopts the presoma as nanometer activated carbon fiber through the bacteria cellulose of special treatment, and through carbonization treatment, activation processing, finally obtains bacteria cellulose base nanometer activated carbon fiber material.In preparation process, keep to greatest extent the original three-dimensional network space structure of bacteria cellulose, utilized its synergistic activation effect of NaOH and potassium hydroxide and fast, efficiently prepare a kind of nanometer activated carbon fiber material with three-dimensional net structure by rational temperature control.Preparation is simple in the present invention, easy to operate, cost is low; the bacteria cellulose base nanometer activated carbon fiber obtaining has good spacial framework, high-specific surface area, even aperture distribution, splendid adsorption capacity and the rate of adsorption, can be applicable to the fields such as bio-medical, environmental protection, wastewater and waste gas treatment.
Accompanying drawing explanation
Fig. 1 is the each group of clearance rate comparison to benzene.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1:
The bacteria cellulose obtaining being fermented by Alcaligenes and Aerobacter is placed in the sodium hydrate aqueous solution thermophilic digestion 30min of 10wt%, and by material freezing 24h at-80 ℃, then vacuumize 24h.
Dried bacteria cellulose material is put under atmosphere furnace nitrogen protection by room temperature and is heated up and be heated to 550 ℃ and carry out carbonization treatment, wherein 100～300 ℃ of interval heating rates are 5 ℃/min, 300～500 ℃ of interval heating rates are 1 ℃/min, and 500～550 ℃ of interval heating rates are 30 ℃/min; Intensification finishes rear material and in atmosphere furnace, slowly cools to room temperature.
The potassium hydroxide aqueous solution of material after carbonization being put into 10wt% soaks 30min, inserts in the activation furnace of nitrogen protection and heat up and be heated to 700 ℃ after oven dry, and temperature retention time is 60min.Insulation finishes rear material and in activation furnace, slowly cools to room temperature and obtain nanofiber diameter and be about 30nm, is evenly distributed with the bacteria cellulose base nanometer activated carbon fiber that diameter is about the micropore of 2nm and has three-dimensional network space structure on fiber.
Embodiment 2:
The bacteria cellulose obtaining being fermented by acetobacter xylinum is placed in the sodium hydrate aqueous solution thermophilic digestion 20min of 15wt%, and by material freezing 24h at-20 ℃, then vacuumize 24h.
Dried bacteria cellulose material is put into atmosphere furnace and is heated up and be heated to 600 ℃ and carry out carbonization treatment by room temperature under vacuum, wherein 100～300 ℃ of interval heating rates are 5 ℃/min, 300～500 ℃ of interval heating rates are 1 ℃/min, and 500～600 ℃ of interval heating rates are 30 ℃/min; Intensification finishes rear material and in atmosphere furnace, slowly cools to room temperature.
The potassium hydroxide aqueous solution of material after carbonization being put into 20wt% soaks 20min, inserts in the activation furnace of nitrogen protection and heat up and be heated to 800 ℃ after oven dry, and temperature retention time is 30min.Insulation finishes rear material and in activation furnace, slowly cools to room temperature and obtain nanofiber diameter and be about 10nm, is evenly distributed with the bacteria cellulose base nanometer activated carbon fiber that diameter is about the micropore of 0.5nm and has three-dimensional network space structure on fiber.
Embodiment 3:
The bacteria cellulose obtaining being fermented by Sarcina and pseudomonas is placed in the sodium hydrate aqueous solution thermophilic digestion 10min of 20wt%, and by material freezing 12h at-30 ℃, then vacuumize 48h.
Dried bacteria cellulose material is put into atmosphere furnace and is heated up and be heated to 560 ℃ and carry out carbonization treatment by room temperature under vacuum, wherein 100～300 ℃ of interval heating rates are 6 ℃/min, 300～500 ℃ of interval heating rates are 2 ℃/min, and 500～560 ℃ of interval heating rates are 30 ℃/min; Intensification finishes rear material and in atmosphere furnace, slowly cools to room temperature.
The potassium hydroxide aqueous solution of material after carbonization being put into 30wt% soaks 10min, inserts in the activation furnace of nitrogen protection and heat up and be heated to 900 ℃ after oven dry, and temperature retention time is 10min.Insulation finishes rear material and in activation furnace, slowly cools to room temperature and obtain nanofiber diameter and be about 15nm, is evenly distributed with the bacteria cellulose base nanometer activated carbon fiber that diameter is about the micropore of 1nm and has three-dimensional network space structure on fiber.
Embodiment 4:
The bacteria cellulose obtaining being fermented by achromobacter and azotobacter is placed in the sodium hydrate aqueous solution thermophilic digestion 20min of 12wt%, and by material freezing 24h at-40 ℃, then vacuumize 24h.
Dried bacteria cellulose material is put under atmosphere furnace argon shield by room temperature and is heated up and be heated to 580 ℃ and carry out carbonization treatment, wherein 100～300 ℃ of interval heating rates are 8 ℃/min, 300～500 ℃ of interval heating rates are 3 ℃/min, and 580 ℃ of interval heating rates are 30 ℃/min; Intensification finishes rear material and in atmosphere furnace, slowly cools to room temperature.
The potassium hydroxide aqueous solution of material after carbonization being put into 30wt% soaks 30min, inserts in the activation furnace of nitrogen protection and heat up and be heated to 700 ℃ after oven dry, and temperature retention time is 20min.Insulation finishes rear material and in activation furnace, slowly cools to room temperature and obtain nanofiber diameter and be about 20nm, is evenly distributed with the bacteria cellulose base nanometer activated carbon fiber that diameter is about the micropore of 1.5nm and has three-dimensional network space structure on fiber.
Embodiment 5:
The bacteria cellulose obtaining being fermented by rhizobium is placed in the sodium hydrate aqueous solution thermophilic digestion 10min of 10wt%, and by material freezing 12h at-80 ℃, then vacuumize 48h.
Dried bacteria cellulose material is put under atmosphere furnace argon shield by room temperature and is heated up and be heated to 600 ℃ and carry out carbonization treatment, wherein 100～300 ℃ of interval heating rates are 10 ℃/min, 300～500 ℃ of interval heating rates are 5 ℃/min, and 500～600 ℃ of interval heating rates are 30 ℃/min; Intensification finishes rear material and in atmosphere furnace, slowly cools to room temperature.
The potassium hydroxide aqueous solution of material after carbonization being put into 20wt% soaks 30min, inserts in the activation furnace of nitrogen protection and heat up and be heated to 800 ℃ after oven dry, and temperature retention time is 40min.Insulation finishes rear material and in activation furnace, slowly cools to room temperature and obtain nanofiber diameter and be about 25nm, is evenly distributed with the bacteria cellulose base nanometer activated carbon fiber that diameter is about the micropore of 1.8nm and has three-dimensional network space structure on fiber.
Experimental example 1: the nanometer activated carbon fiber photo-catalysis capability test of carried titanium dioxide
The bacteria cellulose base nanometer activated carbon fiber of embodiment 1-3 is carried out to carried titanium dioxide crystal operation, be specially: first dried bacteria cellulose material is immersed in the TiO 2 precursor solution that titanium tetraisopropylate mixes with 1:4 volume ratio in absolute ethyl alcohol, ultrasonic processing 30min, and after cleaning with ethanol, then carry out carbonization treatment.
Measure its catalytic activity take methyl orange as simulating pollution thing:
It it is 5 groups by experiment component: group 1: negative control group (commercially available cocoanut active charcoal); Group 2-4: of the present invention group (nano active carbon of carried titanium dioxide prepared by embodiment 1-3); Group 5: positive controls (TiO prepared by Chinese invention patent CN102861563A embodiment 1
2/ AC).Accurately get the beaker that catalyst 0.15g is placed in 150mL, add 5.0 × 10
-5the methyl orange aqueous solution 150mL of g/mL, soaked overnight, wait to reach absorption saturated after, slowly outwell supernatant, then add the methyl orange solution of 25mL same concentrations, be placed at (10cm place) under 40W uviol lamp, open uviol lamp, the degradation rate of the nano active C catalyst of mensuration carried titanium dioxide to methyl orange, light degradation is after 80 minutes, and result is as follows:
The photocatalytic activity of the each catalyst of table 1 to methyl orange
| ? | Negative control group | 1 group of embodiment | 2 groups of embodiment | 3 groups of embodiment | Positive controls |
| Methyl orange degradation rate (%) | 48.6 | 92.3 | 82.1 | 86.2 | 81.5 |
Degradation rate=(concentration of the front methyl orange of the concentration/catalysis of methyl orange after 1-catalysis) × 100% of methyl orange.
Use same catalyst sample by each group, repeat above-mentioned experiment, and the methyl orange degradation rate of the each experiment of record.If this degradation rate and last registration value relatively lower than 2%, continue to repeat.If degradation rate exceedes 2%, stop experiment, record the access times of this sample, result is as following table:
The each catalyst of table 2 is reused number of times comparison
| ? | Negative control group | 1 group of embodiment | 2 groups of embodiment | 3 groups of embodiment | Positive controls |
| Access times | 2 | 13 | 13 | 10 | 7 |
Access times are to use same catalyst to make degradation rate change the number of times that is less than 2%.
Show by above experiment, use the photo-catalysis capability of nanometer activated carbon fiber of the carried titanium dioxide that technical scheme of the present invention prepares the strongest, and be better than common activated carbon sample far away, the catalyst of also preparing higher than prior art.In addition, material recycling degree prepared by the present invention, significantly better than other each group, is reused 10 above degradation rates variations and is all less than 2%, has greatly saved cost, environmental protection.
Experimental example 2: the nanometer activated carbon fiber photo-catalysis capability test 2 of carried titanium dioxide
Measure its catalytic activity take benzene as simulating pollution thing:
It it is 5 groups by experiment component: group 1: negative control group (commercially available cocoanut active charcoal); Group 2-4: of the present invention group (nano active carbon of carried titanium dioxide prepared by embodiment 1-3); Group 5: positive controls (TiO prepared by Chinese invention patent CN102861563A embodiment 1
2/ AC).This experiment adopts batch (-type) light reaction system.1.0g sample is dropped into from the sample tap of quartzy Photoreactor, be evenly distributed on the bottom of reactor; Then system is evacuated, gets a certain amount of benzene liquid with micro syringe, be injected in the quartzy Photoreactor of vacuum state; Be 21% oxygen to being filled with percent by volume in system, 79% nitrogen, makes the pressure of system reach 1.01 × 10
5pa.The quartzy Photoreactor that finite concentration pollutant is housed is put into light reaction case, it is respectively the 8W uviol lamp of 365 nm by dominant wavelength, dominant wavelength is that 8W uviol lamp and the dominant wavelength of 254 nm is the 500W high voltage mercury lamp radiation quartz reactor of 365 nm, and the distance of lamp and quartzy Photoreactor is 20cm.Before each light reaction, first the quartzy Photoreactor dark place that pollutant is housed is left standstill to 40min, then open light source, every 10min, from the sample tap of quartzy Photoreactor, with the airtight pin sampling of 1mL, be injected into and in gas chromatograph, analyze mensuration.
Result is referring to accompanying drawing 1.
From figure, show known, aspect the elimination efficiency for pollutant benzene, 3 groups of embodiment all can remove completely in 50 minutes, and commercially available active carbon and positive control only can be removed part benzene in 60 minutes, and technical scheme of the present invention has shown more excellent effect.
Can find out based on above experiment, through the inventive method, the bacteria cellulose base nanometer activated carbon fiber of acquisition is crossed in special treatment, has good absorption property, can significantly improve the photocatalytic activity of titanium dioxide.
In addition, through relatively finding, compared with prior art, activated carbon fiber prepared by the present invention has higher specific area and micropore porosity, and for example the specific area of viscose glue base, the fine base of polypropylene, phenolic aldehyde base and asphalt activity carbon fiber is respectively 1000-1500m
2/ g, 700-1200m
2/ g, 1000-2300m
2/ g and 1000-2000m
2/ g, and BET result shows, the specific area of the wooden carbon fiber of activity that employing the inventive method makes is 1299.39m
2/ g-2821.62 m
2/ g, micropore porosity is 88%-95%.
Claims (9)
1. a bacteria cellulose base nanometer activated carbon fiber, is characterized in that: make activated carbon fiber by bacteria cellulose, described bacteria cellulose is obtained by bacterial fermentation.
2. the preparation method of a bacteria cellulose base nanometer activated carbon fiber, it is characterized in that: by the bacteria cellulose purification process, the freeze drying that are obtained by bacterial fermentation, then dried bacteria cellulose material is put into atmosphere furnace carbonization treatment and be heated to 550 ℃～600 ℃, the potassium hydroxide aqueous solution of putting into 10～30wt% after material cooled soaks 10～30min, after oven dry, through further activation processing, obtain having the bacteria cellulose base nanometer activated carbon fiber material of three-dimensional net structure after cooling.
3. the preparation method of a kind of bacteria cellulose base nanometer activated carbon fiber as claimed in claim 2, it is characterized in that: described bacterium refers to and can, by the bacterial strain of fermented-producing bacteria cellulose, comprise: one or more in acetobacter xylinum, rhizobium, Sarcina, pseudomonas, achromobacter, Alcaligenes, Aerobacter or azotobacter.
4. the preparation method of a kind of bacteria cellulose base nanometer activated carbon fiber as claimed in claim 2, is characterized in that: described purification process refers to, bacteria cellulose is through sodium hydrate aqueous solution thermophilic digestion 10～30min of 10～20wt%.
5. the preparation method of a kind of bacteria cellulose base nanometer activated carbon fiber as claimed in claim 2, it is characterized in that: described freeze drying refers to the bacteria cellulose after purification process freezing 12～24h, then vacuumize 24～48h at-20 ℃～-80 ℃.
6. the preparation method of a kind of bacteria cellulose base nanometer activated carbon fiber as claimed in claim 2; it is characterized in that: described carbonization treatment refers to that bacteria cellulose material is under vacuum, argon gas or nitrogen protection; be warming up to 550 ℃～600 ℃ by room temperature; wherein 100～300 ℃ of interval heating rates are 5～10 ℃/min; 300～500 ℃ of interval heating rates are 1～5 ℃/min, and 500～600 ℃ of interval heating rates are 30 ℃/min.
7. the preparation method of a kind of bacteria cellulose base nanometer activated carbon fiber as claimed in claim 2; it is characterized in that: described activity processing refer to potassium hydroxide aqueous solution soak after material put into nitrogen protection activation furnace heat up heating; heating-up temperature is 700～900 ℃, and temperature retention time is 10～60min.
8. the preparation method of a kind of bacteria cellulose base nanometer activated carbon fiber as claimed in claim 2, is characterized in that: described coolingly refer to that the bacteria cellulose material heating up after finishing slowly cools to room temperature in atmosphere furnace or activation furnace.
9. the preparation method of a kind of bacteria cellulose base nanometer activated carbon fiber as claimed in claim 2, it is characterized in that: described bacteria cellulose base nanometer activated carbon fiber material refers to that activated carbon fiber diameter is about 10～30nm, is evenly distributed with 0.5～2nm micropore and has three-dimensional network space structure on fiber.
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