CN103806130B - A kind of preparation method of bacteria cellulose-base nanometer activated carbon fiber - Google Patents
A kind of preparation method of bacteria cellulose-base nanometer activated carbon fiber Download PDFInfo
- Publication number
- CN103806130B CN103806130B CN201410063237.4A CN201410063237A CN103806130B CN 103806130 B CN103806130 B CN 103806130B CN 201410063237 A CN201410063237 A CN 201410063237A CN 103806130 B CN103806130 B CN 103806130B
- Authority
- CN
- China
- Prior art keywords
- bacteria cellulose
- activated carbon
- carbon fiber
- room temperature
- base nanometer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The invention discloses a kind of preparation method of bacteria cellulose-base nanometer activated carbon fiber.Relate to a kind of active carbon material technology of preparing.Comprise: by obtained by bacterial fermentation bacteria cellulose purification process, freeze drying, then dried bacteria cellulose material is put into atmosphere furnace carbonization treatment and be heated to 550 DEG C ~ 600 DEG C, put into potassium hydroxide aqueous solution after material cooled and soak 10 ~ 30min, through further activation processing after oven dry, after cooling, obtain the bacteria cellulose-base nanometer activated carbon fiber material with 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 obtained has good spacial framework, high-specific surface area, splendid adsorption capacity and the rate of adsorption; desorption is convenient, can be applicable to the fields such as bio-medical, environmental protection, wastewater and waste gas treatment.
Description
Technical field
The present invention relates to active carbon material field, refers to a kind of preparation method of bacteria cellulose-base nanometer activated carbon fiber especially.
Background technology
Activated carbon is a kind of porous carbon through activation processing, has extremely strong adsorption capacity, has century-old history in the application in the 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 physical aspect makes itself and adsorbate have larger contact area, thus 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 the various products such as felt, cloth, paper as required, more flexible during use.Therefore, the application of activated carbon fiber in chemical industry, environmental protection, electronics industry, medical, food hygiene etc. more and more receives the concern of people.
Carbon nano-fiber refers to the activated carbon fiber with nanoscale, many performance basis of activated carbon fiber add nano effect, nanometer activated carbon fiber is made to have 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 nanometer, and is intertwined to form flourishing hyperfine network structure.The characteristic of the high-purity of bacteria cellulose, high-crystallinity, high polymerization degree and numberator height orientation, makes it have the primary condition becoming nanometer activated carbon fiber presoma.
This patent adopts bacteria cellulose through special treatment as the presoma of nanometer activated carbon fiber, and through carbonization treatment, activation processing, finally obtains the nanometer activated carbon fiber material with 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 obtained 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 obtained 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 disclosing a kind of bacteria cellulose-base nanometer activated carbon fiber of the present invention, comprise: by obtained by bacterial fermentation bacteria cellulose purification process, freeze drying, then dried bacteria cellulose material is put into atmosphere furnace carbonization treatment and be heated to 550 DEG C ~ 600 DEG C, the potassium hydroxide aqueous solution putting into 10 ~ 30wt% after material cooled soaks 10 ~ 30min, through further activation processing after oven dry, after cooling, obtain the bacteria cellulose-base nanometer activated carbon fiber material with three-dimensional net structure.
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 the bacterial strain by fermented-producing bacteria cellulose, comprising: 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 the sodium hydrate aqueous solution thermophilic digestion 10 ~ 30min of 10 ~ 20wt%.In the bacteria cellulose raw material of bacterial fermentation, have a large amount of bacterium Remained mass, material is formed local defect by these residues in the process of carbonization, activation, has a strong impact on porous aperture and the three-dimensional net structure of the nanometer activated carbon fiber obtained.Sodium hydroxide solution boiling thoroughly can be removed mycoprotein and be sticked to the residual media on cellulose membrane, ensures 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 freezing 12 ~ 24h at-20 DEG C ~-80 DEG C of the bacteria cellulose after by purification process, then vacuumize 24 ~ 48h.Freeze drying object is three-dimensional network microstructure when maintaining 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; by room temperature to 550 DEG C ~ 600 DEG C; wherein 100 ~ 300 DEG C of interval heating rates are 5 ~ 10 DEG C/min; 300 ~ 500 DEG C of interval heating rates are 1 ~ 5 DEG C/min, and 500 ~ 600 DEG C of interval heating rates are 30 DEG C/min.In this patent, calefactive interzone is divided into three sections of controls, 100 ~ 300 DEG C of intervals are mainly bacteria cellulose and lose physical absorption water, Hydrogenbond water and intermolecular hydrogen bonding, intramolecular hydrogen bond fracture decomposition; 300 ~ 500 DEG C of intervals are mainly the fracture of bacteria cellulose carbochain and decompose, and generate a small amount of volatilization gas.These two calefactive interzones are keys of material carbonisation, and in bacteria cellulose carbonisation, quality can significantly reduce, and volume can along with contraction.In the meantime in order to maintain the original three-dimensional net structure of bacteria cellulose, strictly must control the heating rate of carbonisation, preventing 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; the activation furnace intensification heating of nitrogen protection put into by material after described activation processing refers to potassium hydroxide aqueous solution immersion; heating-up temperature is 700 ~ 900 DEG C, and temperature retention time is 10 ~ 60min.With the carbon fiber that potassium hydroxide aqueous solution soaked, along with the evaporation of fibrous inside steam in heating process, some potassium hydroxide granules be evenly distributed can be gone out in fiber surface crystallization, when activating treatment temperature raises, these granule original positions and carbon react, 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, plays facilitation to the activation of whole carbon fiber.In like manner, residual in bacteria cellulose purification process process NaOH also has the identical active effect of potassium hydroxide.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 cooling refers to that the bacteria cellulose material after terminating that heats up 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, fiber is evenly distributed with 0.5 ~ 2nm micropore and has three-dimensional network space structure.
Compared with prior art, the invention has the beneficial effects as follows:
The present invention adopts bacteria cellulose through special treatment as the presoma of nanometer activated carbon fiber, and through carbonization treatment, activation processing, finally obtains bacteria cellulose-base nanometer activated carbon fiber material.In preparation process, maintain the original three-dimensional network space structure of bacteria cellulose to greatest extent, utilize its synergistic activation effect of NaOH and potassium hydroxide and control fast, efficiently to prepare a kind of nanometer activated carbon fiber material with three-dimensional net structure by rational temperature.Preparation is simple in the present invention, easy to operate, cost is low; the bacteria cellulose-base nanometer activated carbon fiber obtained 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 each group and compares the clearance rate of benzene.
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1:
The bacteria cellulose obtained 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 DEG C, then vacuumize 24h.
Dried bacteria cellulose material is heated to 550 DEG C by room temperature under putting into atmosphere furnace nitrogen protection and carries out carbonization treatment, wherein 100 ~ 300 DEG C of interval heating rates are 5 DEG C/min, 300 ~ 500 DEG C of interval heating rates are 1 DEG C/min, and 500 ~ 550 DEG C of interval heating rates are 30 DEG C/min; Intensification terminates rear material and slowly cool to room temperature in atmosphere furnace.
The potassium hydroxide aqueous solution that 10wt% put into by material after carbonization is soaked 30min, and inserting after oven dry in the activation furnace of nitrogen protection heats up is heated to 700 DEG C, and temperature retention time is 60min.Insulation terminates rear material and in activation furnace, slowly cools to room temperature obtain nanofiber diameter and be about 30nm, fiber is evenly distributed with diameter and is about the micropore of 2nm and has the bacteria cellulose-base nanometer activated carbon fiber of three-dimensional network space structure.
Embodiment 2:
The bacteria cellulose obtained 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 DEG C, then vacuumize 24h.
Dried bacteria cellulose material is put into atmosphere furnace and is heated to 600 DEG C by room temperature under vacuo and carries out carbonization treatment, wherein 100 ~ 300 DEG C of interval heating rates are 5 DEG C/min, 300 ~ 500 DEG C of interval heating rates are 1 DEG C/min, and 500 ~ 600 DEG C of interval heating rates are 30 DEG C/min; Intensification terminates rear material and slowly cool to room temperature in atmosphere furnace.
The potassium hydroxide aqueous solution that 20wt% put into by material after carbonization is soaked 20min, and inserting after oven dry in the activation furnace of nitrogen protection heats up is heated to 800 DEG C, and temperature retention time is 30min.Insulation terminates rear material and in activation furnace, slowly cools to room temperature obtain nanofiber diameter and be about 10nm, fiber is evenly distributed with diameter and is about the micropore of 0.5nm and has the bacteria cellulose-base nanometer activated carbon fiber of three-dimensional network space structure.
Embodiment 3:
The bacteria cellulose obtained 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 DEG C, then vacuumize 48h.
Dried bacteria cellulose material is put into atmosphere furnace and is heated to 560 DEG C by room temperature under vacuo and carries out carbonization treatment, wherein 100 ~ 300 DEG C of interval heating rates are 6 DEG C/min, 300 ~ 500 DEG C of interval heating rates are 2 DEG C/min, and 500 ~ 560 DEG C of interval heating rates are 30 DEG C/min; Intensification terminates rear material and slowly cool to room temperature in atmosphere furnace.
The potassium hydroxide aqueous solution that 30wt% put into by material after carbonization is soaked 10min, and inserting after oven dry in the activation furnace of nitrogen protection heats up is heated to 900 DEG C, and temperature retention time is 10min.Insulation terminates rear material and in activation furnace, slowly cools to room temperature obtain nanofiber diameter and be about 15nm, fiber is evenly distributed with diameter and is about the micropore of 1nm and has the bacteria cellulose-base nanometer activated carbon fiber of three-dimensional network space structure.
Embodiment 4:
The bacteria cellulose obtained 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 DEG C, then vacuumize 24h.
Dried bacteria cellulose material is heated to 580 DEG C by room temperature under putting into atmosphere furnace argon shield and carries out carbonization treatment, wherein 100 ~ 300 DEG C of interval heating rates are 8 DEG C/min, 300 ~ 500 DEG C of interval heating rates are 3 DEG C/min, and 580 DEG C of interval heating rates are 30 DEG C/min; Intensification terminates rear material and slowly cool to room temperature in atmosphere furnace.
The potassium hydroxide aqueous solution that 30wt% put into by material after carbonization is soaked 30min, and inserting after oven dry in the activation furnace of nitrogen protection heats up is heated to 700 DEG C, and temperature retention time is 20min.Insulation terminates rear material and in activation furnace, slowly cools to room temperature obtain nanofiber diameter and be about 20nm, fiber is evenly distributed with diameter and is about the micropore of 1.5nm and has the bacteria cellulose-base nanometer activated carbon fiber of three-dimensional network space structure.
Embodiment 5:
The bacteria cellulose obtained being fermented by rhizobium is placed in the sodium hydrate aqueous solution thermophilic digestion 10min of 10wt%, and by material freezing 12h at-80 DEG C, then vacuumize 48h.
Dried bacteria cellulose material is heated to 600 DEG C by room temperature under putting into atmosphere furnace argon shield and carries out carbonization treatment, wherein 100 ~ 300 DEG C of interval heating rates are 10 DEG C/min, 300 ~ 500 DEG C of interval heating rates are 5 DEG C/min, and 500 ~ 600 DEG C of interval heating rates are 30 DEG C/min; Intensification terminates rear material and slowly cool to room temperature in atmosphere furnace.
The potassium hydroxide aqueous solution that 20wt% put into by material after carbonization is soaked 30min, and inserting after oven dry in the activation furnace of nitrogen protection heats up is heated to 800 DEG C, and temperature retention time is 40min.Insulation terminates rear material and in activation furnace, slowly cools to room temperature obtain nanofiber diameter and be about 25nm, fiber is evenly distributed with diameter and is about the micropore of 1.8nm and has the bacteria cellulose-base nanometer activated carbon fiber of three-dimensional network space structure.
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 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 process 30min, and with after ethanol purge, then carry out carbonization treatment.
Be that simulating pollution thing measures its catalytic activity with methyl orange:
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: the positive controls (TiO of Chinese invention patent CN102861563A embodiment 1 preparation
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, after absorption to be achieved is saturated, slowly outwell supernatant, then add the methyl orange solution of 25mL same concentrations, under being placed on 40W uviol lamp (10cm place), open uviol lamp, measure the nano active C catalyst of carried titanium dioxide to the degradation rate of methyl orange, light degradation is after 80 minutes, and result is as follows:
The each catalyst of table 1 is to the photocatalytic activity of methyl orange
| Negative control group | Embodiment 1 group | Embodiment 2 groups | Embodiment 3 groups | Positive controls | |
| Methyl orange degradation rate (%) | 48.6 | 92.3 | 82.1 | 86.2 | 81.5 |
The degradation rate of methyl orange=(after 1-catalysis methyl orange concentration/catalysis before the concentration of methyl orange) × 100%.
Use same catalyst sample by each group, repeat above-mentioned experiment, and the methyl orange degradation rate of each experiment of record.If this degradation rate compares lower than 2% with last registration value, then continue repetition.If degradation rate is more than 2%, then 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 and is compared
| Negative control group | Embodiment 1 group | Embodiment 2 groups | Embodiment 3 groups | Positive controls | |
| Access times | 2 | 13 | 13 | 10 | 7 |
Access times are use same catalyst to make degradation rate change the number of times being less than 2%.
Show by testing above, the photo-catalysis capability of the nanometer activated carbon fiber of the carried titanium dioxide using technical scheme of the present invention to prepare is the strongest, and is better than common activated carbon sample far away, also higher than catalyst prepared by prior art.In addition, material recycling degree prepared by the present invention is significantly better than other each group, and the degradation rate change reusing more than 10 times 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
Be that simulating pollution thing measures its catalytic activity with benzene:
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: the positive controls (TiO of Chinese invention patent CN102861563A embodiment 1 preparation
2/ AC).This experiment adopts batch (-type) light reaction system.The sample tap of 1.0g sample from quartzy Photoreactor is dropped into, is 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; In system, be filled with the oxygen that percent by volume is 21%, the nitrogen of 79%, make the pressure of system reach 1.01 × 10
5pa.The quartzy Photoreactor that finite concentration pollutant is housed is put into light reaction case, be the 8W uviol lamp of 365nm respectively by dominant wavelength, the 500W high voltage mercury lamp radiation quartz reactor of dominant wavelength to be the 8W uviol lamp of 254nm and dominant wavelength be 365nm, 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 40min, then open light source, every 10min, from the sample tap of quartzy Photoreactor, with the airtight pin sampling of 1mL, be injected in gas chromatograph and carry out analysis mensuration.
Result is see accompanying drawing 1.
Show known from figure, in the elimination efficiency for pollutant benzene, 3 groups of embodiments all can be removed completely in 50 minutes, and commercially available active carbon and positive control only can remove part benzene in 60 minutes, and technical scheme of the present invention shows more excellent effect.
Can find out based on above experiment, cross the bacteria cellulose-base nanometer activated carbon fiber of acquisition through the inventive method special treatment, there is good absorption property, the photocatalytic activity of titanium dioxide can be significantly improved.
In addition, through comparing discovery, compared with prior art, activated carbon fiber prepared by the present invention has higher specific area and micropore rate, and such as 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 adopting the inventive method to obtain is 1299.39m
2/ g-2821.62m
2/ g, micropore rate is 88%-95%.
Claims (3)
1. the preparation method of a bacteria cellulose-base nanometer activated carbon fiber, it is characterized in that: the bacteria cellulose obtained 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 DEG C, then vacuumize 24h; Dried bacteria cellulose material is heated to 550 DEG C by room temperature under putting into atmosphere furnace nitrogen protection and carries out carbonization treatment, wherein 100 ~ 300 DEG C of interval heating rates are 5 DEG C/min, 300 ~ 500 DEG C of interval heating rates are 1 DEG C/min, and 500 ~ 550 DEG C of interval heating rates are 30 DEG C/min; Intensification terminates rear material and slowly cool to room temperature in atmosphere furnace; The potassium hydroxide aqueous solution that 10wt% put into by material after carbonization is soaked 30min, and inserting after oven dry in the activation furnace of nitrogen protection heats up is heated to 700 DEG C, and temperature retention time is 60min; Insulation terminates rear material and in activation furnace, slowly cools to room temperature to obtain nanofiber diameter be 30nm, fiber is evenly distributed with micropore that diameter is 2nm and has the bacteria cellulose-base nanometer activated carbon fiber of three-dimensional network space structure.
2. the preparation method of a bacteria cellulose-base nanometer activated carbon fiber, it is characterized in that: the bacteria cellulose obtained 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 DEG C, then vacuumize 24h; Dried bacteria cellulose material is put into atmosphere furnace and is heated to 600 DEG C by room temperature under vacuo and carries out carbonization treatment, wherein 100 ~ 300 DEG C of interval heating rates are 5 DEG C/min, 300 ~ 500 DEG C of interval heating rates are 1 DEG C/min, and 500 ~ 600 DEG C of interval heating rates are 30 DEG C/min; Intensification terminates rear material and slowly cool to room temperature in atmosphere furnace; The potassium hydroxide aqueous solution that 20wt% put into by material after carbonization is soaked 20min, and inserting after oven dry in the activation furnace of nitrogen protection heats up is heated to 800 DEG C, and temperature retention time is 30min; Insulation terminates rear material and in activation furnace, slowly cools to room temperature to obtain nanofiber diameter be 10nm, fiber is evenly distributed with micropore that diameter is 0.5nm and has the bacteria cellulose-base nanometer activated carbon fiber of three-dimensional network space structure.
3. the preparation method of a bacteria cellulose-base nanometer activated carbon fiber, it is characterized in that: the bacteria cellulose obtained 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 DEG C, then vacuumize 48h; Dried bacteria cellulose material is put into atmosphere furnace and is heated to 560 DEG C by room temperature under vacuo and carries out carbonization treatment, wherein 100 ~ 300 DEG C of interval heating rates are 6 DEG C/min, 300 ~ 500 DEG C of interval heating rates are 2 DEG C/min, and 500 ~ 560 DEG C of interval heating rates are 30 DEG C/min; Intensification terminates rear material and slowly cool to room temperature in atmosphere furnace; The potassium hydroxide aqueous solution that 30wt% put into by material after carbonization is soaked 10min, and inserting after oven dry in the activation furnace of nitrogen protection heats up is heated to 900 DEG C, and temperature retention time is 10min; Insulation terminates rear material and in activation furnace, slowly cools to room temperature to obtain nanofiber diameter be 15nm, fiber is evenly distributed with micropore that diameter is 1nm and has the bacteria cellulose-base nanometer activated carbon fiber of three-dimensional network space structure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410063237.4A CN103806130B (en) | 2014-02-24 | 2014-02-24 | A kind of preparation method of bacteria cellulose-base nanometer activated carbon fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410063237.4A CN103806130B (en) | 2014-02-24 | 2014-02-24 | A kind of preparation method of bacteria cellulose-base nanometer activated carbon fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103806130A CN103806130A (en) | 2014-05-21 |
| CN103806130B true CN103806130B (en) | 2016-02-10 |
Family
ID=50703494
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410063237.4A Active CN103806130B (en) | 2014-02-24 | 2014-02-24 | A kind of preparation method of bacteria cellulose-base nanometer activated carbon fiber |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103806130B (en) |
Families Citing this family (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103966700B (en) * | 2014-05-27 | 2016-03-30 | 哈尔滨工业大学 | Bacteria cellulose is utilized to prepare the method for carbon nano-fiber aeroge oil absorption material |
| CN105140042B (en) * | 2015-09-08 | 2017-11-14 | 哈尔滨工业大学 | A kind of preparation method and applications of bacteria cellulose/activated carbon fiber/CNT membrane material |
| CN105036131A (en) * | 2015-09-08 | 2015-11-11 | 哈尔滨工业大学 | Preparing method of nanometer active carbon fiber |
| CN105174253A (en) * | 2015-09-08 | 2015-12-23 | 哈尔滨工业大学 | Method for preparing nano active carbon fiber in one step |
| CN106587006B (en) * | 2016-11-18 | 2019-01-22 | 浙江理工大学 | A method of carbon nano rod is prepared based on Cellulose nanocrystal |
| CN107200332B (en) * | 2017-06-07 | 2019-04-05 | 南京宝淳新材料科技有限公司 | A kind of preparation method of nano silica |
| CN110997563B (en) * | 2017-08-04 | 2023-01-13 | 日本电信电话株式会社 | Cellulose nanofiber carbon and method for producing same |
| JP7048889B2 (en) * | 2018-04-16 | 2022-04-06 | 日本電信電話株式会社 | Method for producing bacterially produced cellulose carbon |
| CN108579436A (en) * | 2018-04-28 | 2018-09-28 | 蒋春霞 | A kind of preparation method of gradient duct carbon microfiltration membrane |
| CN109772363B (en) * | 2019-03-28 | 2020-10-27 | 中国科学技术大学 | Carbon nanofiber solid acid catalyst, preparation method thereof and application of carbon nanofiber solid acid catalyst in catalytic reaction |
| WO2020220300A1 (en) * | 2019-04-30 | 2020-11-05 | 钟春燕 | Biocellulose fiber, hemostatic dressing comprising said fiber and related application |
| CN110485001B (en) * | 2019-08-05 | 2022-03-18 | 武汉纺织大学 | Method for preparing activated carbon fiber based on centrifugal spinning method |
| CN112553883B (en) * | 2019-09-25 | 2023-02-10 | 钟春燕 | Biocellulosic fibres, hemostatic dressings comprising said fibres and related applications |
| CN110844903B (en) * | 2019-11-25 | 2021-04-27 | 西北大学 | Preparation method of bacterial cellulose-based composite porous carbon material |
| CN111591972B (en) * | 2020-05-18 | 2022-12-23 | 华东交通大学 | Super-elastic hydrophilic all-carbon aerogel and preparation method thereof |
| CN113562730A (en) * | 2021-03-11 | 2021-10-29 | 海南师范大学 | Preparation of microporous gram bacteria carbon material with high specific surface area and application of microporous gram bacteria carbon material in supercapacitor |
| CN114293364B (en) * | 2022-01-28 | 2023-09-26 | 华北电力大学（保定） | Carbon fiber activation method and equipment |
| CN116986788B (en) * | 2023-09-26 | 2024-01-12 | 深圳市深水水务咨询有限公司 | Efficient multifunctional sludge conditioner and preparation method thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009074183A (en) * | 2007-09-19 | 2009-04-09 | Toray Ind Inc | Heat treatment furnace and method for producing carbon fiber using the same |
| CN103184651A (en) * | 2011-12-31 | 2013-07-03 | 中原工学院 | Preparation method of bacteria cellulose fiber-based carbon nanofiber knitted fabric |
| CN103184586A (en) * | 2011-12-31 | 2013-07-03 | 中原工学院 | Preparation method of bacterial-cellulose-fiber-based nano-grade carbon fiber |
| CN103184655A (en) * | 2011-12-31 | 2013-07-03 | 中原工学院 | Preparation method of bacteria cellulose fiber-based carbon nanofiber non-woven fabric |
| CN103184621A (en) * | 2011-12-31 | 2013-07-03 | 中原工学院 | Preparation method of bacteria cellulose fiber-based carbon nanofiber woven cloth |
| CN103184602A (en) * | 2011-12-31 | 2013-07-03 | 中原工学院 | Preparation method of bacteria cellulose fiber-based carbon nanofiber thread |
| CN103184601A (en) * | 2011-12-31 | 2013-07-03 | 中原工学院 | Preparation method of bacteria cellulose fiber-based carbon nanofiber yarn |
| CN103409853A (en) * | 2013-08-22 | 2013-11-27 | 吉林大学 | Method for preparing active carbon fiber material with energy storage characteristic from polyacrylonitrile-based pre-oxidized fiber and application of active carbon fiber material |
-
2014
- 2014-02-24 CN CN201410063237.4A patent/CN103806130B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009074183A (en) * | 2007-09-19 | 2009-04-09 | Toray Ind Inc | Heat treatment furnace and method for producing carbon fiber using the same |
| CN103184651A (en) * | 2011-12-31 | 2013-07-03 | 中原工学院 | Preparation method of bacteria cellulose fiber-based carbon nanofiber knitted fabric |
| CN103184586A (en) * | 2011-12-31 | 2013-07-03 | 中原工学院 | Preparation method of bacterial-cellulose-fiber-based nano-grade carbon fiber |
| CN103184655A (en) * | 2011-12-31 | 2013-07-03 | 中原工学院 | Preparation method of bacteria cellulose fiber-based carbon nanofiber non-woven fabric |
| CN103184621A (en) * | 2011-12-31 | 2013-07-03 | 中原工学院 | Preparation method of bacteria cellulose fiber-based carbon nanofiber woven cloth |
| CN103184602A (en) * | 2011-12-31 | 2013-07-03 | 中原工学院 | Preparation method of bacteria cellulose fiber-based carbon nanofiber thread |
| CN103184601A (en) * | 2011-12-31 | 2013-07-03 | 中原工学院 | Preparation method of bacteria cellulose fiber-based carbon nanofiber yarn |
| CN103409853A (en) * | 2013-08-22 | 2013-11-27 | 吉林大学 | Method for preparing active carbon fiber material with energy storage characteristic from polyacrylonitrile-based pre-oxidized fiber and application of active carbon fiber material |
Non-Patent Citations (1)
| Title |
|---|
| 细菌纤维素基纳米碳纤维的制备及其储锂储氢性能研究;魏一忠;《天津大学硕士学位论文》;20100630;第16页2.2.1、第17页2.2.2 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103806130A (en) | 2014-05-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103806130B (en) | A kind of preparation method of bacteria cellulose-base nanometer activated carbon fiber | |
| CN103816884B (en) | A kind of nanometer activated carbon fiber preparation method of carried titanium dioxide | |
| Ooi et al. | Conversion and characterization of activated carbon fiber derived from palm empty fruit bunch waste and its kinetic study on urea adsorption | |
| Ahmed et al. | Activated carbon preparation from biomass feedstock: clean production and carbon dioxide adsorption | |
| Hou et al. | Hydrothermal conversion of bamboo shoot shell to biochar: Preliminary studies of adsorption equilibrium and kinetics for rhodamine B removal | |
| Li et al. | Ultrahigh-surface-area activated carbon aerogels derived from glucose for high-performance organic pollutants adsorption | |
| Huang et al. | Surface modification of activated carbon fiber by low-temperature oxygen plasma: Textural property, surface chemistry, and the effect of water vapor adsorption | |
| Sun et al. | Characterization and ciprofloxacin adsorption properties of activated carbons prepared from biomass wastes by H3PO4 activation | |
| Jiao et al. | Synthesis of carbon fiber aerogel from natural bamboo fiber and its application as a green high-efficiency and recyclable adsorbent | |
| Cheng et al. | Hierarchical porous carbon fabricated from cellulose-degrading fungus modified rice husks: Ultrahigh surface area and impressive improvement in toluene adsorption | |
| Gong et al. | An efficient way to introduce hierarchical structure into biomass-based hydrothermal carbonaceous materials | |
| Chen et al. | Dye removal of activated carbons prepared from NaOH-pretreated rice husks by low-temperature solution-processed carbonization and H3PO4 activation | |
| CN107362788B (en) | Graphene oxide/titanium dioxide-activated carbon three-dimensional composite material and preparation method thereof | |
| Wang et al. | Honeycomb-like cork activated carbon with ultra-high adsorption capacity for anionic, cationic and mixed dye: Preparation, performance and mechanism | |
| CN104250003B (en) | A kind of preparation method of nitrogen doping porous carbon nanometer sheet | |
| Gan et al. | Hierarchical porous biochar from plant-based biomass through selectively removing lignin carbon from biochar for enhanced removal of toluene | |
| CN103820883B (en) | A kind of preparation method of bacteria cellulose base nano carbon fibre | |
| Zhang et al. | Microporous carbon nanoflakes derived from biomass cork waste for CO2 capture | |
| Danish et al. | Characterization of physically activated acacia mangium wood-based carbon for the removal of methyl orange dye | |
| CN104722281B (en) | A kind of nano titanium oxide/chitosan three-dimensional is composite porous and preparation method thereof | |
| CN103193228B (en) | Efficient adsorption CO 2the preparation method of melon-seed hull matrix activated carbon | |
| Reza et al. | Analysis on preparation, application, and recycling of activated carbon to aid in COVID-19 protection | |
| CN108043359A (en) | A kind of lignin-degrading bacteria is modified lotus leaf and prepares the method for multi-stage porous charcoal and the application of the multi-stage porous charcoal | |
| Gao et al. | Coal tar residues based activated carbon: Preparation and characterization | |
| Zhang et al. | Preparation of hierarchical porous carbons from sodium carboxymethyl cellulose via halloysite template strategy coupled with KOH-activation for efficient removal of chloramphenicol |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |