CN109972235A - A kind of preparation method of activated carbon fiber - Google Patents
A kind of preparation method of activated carbon fiber Download PDFInfo
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- CN109972235A CN109972235A CN201910221998.0A CN201910221998A CN109972235A CN 109972235 A CN109972235 A CN 109972235A CN 201910221998 A CN201910221998 A CN 201910221998A CN 109972235 A CN109972235 A CN 109972235A
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- Prior art keywords
- activated carbon
- carbon fiber
- preparation
- fiber according
- phosphate
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/16—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from products of vegetable origin or derivatives thereof, e.g. from cellulose acetate
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/68—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
- D06M11/70—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
- D06M11/71—Salts of phosphoric acids
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Carbon And Carbon Compounds (AREA)
- Inorganic Fibers (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The present invention provides a kind of preparation method of activated carbon fiber, it the steps include: for cotton linter to be impregnated in phosphate solution, then dry, be carbonized under nitrogen protection, then activated carbon fiber is obtained with steam activation.The present invention is using cotton linter as raw material, it is not necessary to carry out purification or biological treatment to raw material, preparation process is simple and fast, low production cost, obtained activated carbon fiber specific surface area with higher, can be used for waste water absorption, and can reuse.
Description
Technical field
The present invention relates to a kind of preparation methods of activated carbon fiber, belong to activated carbon fiber preparation technical field.
Technical background
Activated carbon fiber is very promising efficient absorption material, and large specific surface area, there are a large amount of phases in inside
The mutually complicated microcellular structure of perforation.Not only high temperature resistant, corrosion-resistant and conductive, environment compatibility, the small power of regeneration of pollution
Strong to wait excellent performances, no matter polluter is trace level or high concentration, and activated carbon fiber all can be used and carry out adsorption treatment, reach
To promising result, active carbon can be replaced in many fields.
Cotton linter is the very short fiber peeled from the cotton seed surface after cotton ginning, is the important original for extracting pure cotton fiber element
Material.China's cotton linter resource is very rich, and Chinese patent CN102220665A, which was once reported, is prepared high ratio using cotton linter
The activated carbon fiber of surface area, but the method that the patent uses needs to carry out cotton linter Biological Pretreatment to remove non-cellulose
Substance, but also need to use the highly basic of molten condition under high temperature as activator.Time-consuming for this method, in Biological Pretreatment
Stage needs to ferment 4-6 days, and is corroded also very seriously using the highly basic of high-temperature fusion to equipment.The work being prepared by the technology
Although property carbon fiber specific surface area can achieve 2000m2/ g, but preparation process is cumbersome, it is stringent to equipment requirement.
Summary of the invention
For above-mentioned problems of the prior art, activity is prepared using cotton linter the object of the present invention is to provide a kind of
The method of carbon fiber, the method is simple and fast, and gained activated carbon fiber has biggish specific surface area, and adsorption effect is excellent,
It can be used for waste water from dyestuff adsorbing domain.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of preparation method of activated carbon fiber, which comprises the following steps:
(1) cotton linter is immersed in phosphate solution after a period of time, takes out drying, obtains the cotton linter of drying；
(2) under nitrogen protection, the cotton linter by the drying that step (1) obtains is put into tube furnace, is carbonized, is obtained carbon
Intermediate after change；
(3) continue under nitrogen protection, be warming up to certain temperature, be passed through vapor, to the intermediate after the carbonization into
Row activation dries after product is cooling, obtains the activated carbon fibre.
According to the above scheme, it is preferable that the time of dipping described in step (1) is 60~180min.
According to the above scheme, it is preferable that phosphate solution described in step (1) is ammonium hydrogen phosphate, ammonium dihydrogen phosphate, phosphoric acid hydrogen
One or more of potassium, dibastic sodium phosphate, potassium dihydrogen phosphate, sodium dihydrogen phosphate.
According to the above scheme, it is preferable that the concentration of phosphate solution described in step (1) is 1%~10%.
According to the above scheme, it is preferable that the temperature of drying described in step (1) is 30~60 DEG C.
According to the above scheme, it is preferable that the temperature of carbonization described in step (2) is 425 DEG C.
According to the above scheme, it is preferable that the time of carbonization described in step (2) is 30~120min.
According to the above scheme, it is preferable that the rate of heating described in step (3) is 6~12 DEG C/min.
According to the above scheme, it is preferable that certain temperature described in step (3) is 700~1000 DEG C.
According to the above scheme, it is preferable that the time of activation described in step (3) is 30~150min.
According to the above scheme, it is preferable that dried described in step (3) specifically: under the conditions of 60 DEG C, be dried in vacuo 12h.
Compared with prior art, the beneficial effects of the present invention are:
(1) present invention is directly raw material using cotton linter, does not need to carry out Biological Pretreatment to it.Therefore, energy of the present invention
It is enough to utilize raw material to greatest extent, increase the utilization rate of biomass, while simplifying processing step, shortens the process time.
(2) traditional active carbon activating process uses highly basic as activator, and in contrast, the present invention first uses low concentration
Phosphate solution processing cotton linter after, then using vapor as activator, no pollution to the environment, to equipment without particular/special requirement.
(3) activated carbon fiber of the method for the present invention preparation has biggish specific surface area, can reach 1524.09m2/ g, it is empty
Gap is flourishing, and pore-size distribution is concentrated；Suction-operated is strong, function admirable, and may be reused.
Detailed description of the invention
Fig. 1 is the stereoscan photograph of activated carbon fiber obtained in the embodiment of the present invention 1.
Fig. 2 is the nitrogen Adsorption and desorption isotherms of activated carbon fiber obtained in the embodiment of the present invention 1.
Fig. 3 is the graph of pore diameter distribution of activated carbon fiber obtained in the embodiment of the present invention 1.
Fig. 4 is activated carbon fiber obtained in the embodiment of the present invention 1 to Congo red adsorption curve.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..Raw materials used is commercially available quotient
Product.
Embodiment 1
The preparation of activated carbon fiber, the specific steps are as follows:
Cotton linter is immersed in 5% ammonium dihydrogen phosphate, drying is taken out after 1h；Then by the cotton linter after drying
It is put into tube furnace, under the protection of nitrogen, first carries out carbonization-activation, 425 DEG C of carbonization 60min；Then with the rate of 8 DEG C/min
900 DEG C are warming up to, steam activation 30min is passed through；It is taken out after product natural cooling, is put into vacuum oven, it is dry in 60 DEG C
Dry 12h, obtains activated carbon fiber.
The electron microscopic picture of the resulting activated carbon fiber of the present embodiment is as shown in Figure 1.As can be seen from the figure: prepared work
Property carbon fiber surface have different degrees of bumps, it is seen that activation is complete.Uneven is the vapor etching carbon material in activation
Pars amorpha and class graphite microcrystal interface or defect part formed, to form hole.
The nitrogen Adsorption and desorption isotherms of activated carbon fiber obtained are as shown in Fig. 2, it can be seen from the figure that work as in the present embodiment
It interacts when relative pressure increases by zero, between activated carbon fiber and nitrogen strong, adsorbance quicklys increase, with activated carbon
Fiber surface is full of by nitrogen monolayer, reaches saturation state, and adsorption rate does not continue to increase.Adsorption isotherm in figure and de-
Attached thermoisopleth is almost overlapped, and illustrates that the activated carbon fiber of preparation has a large amount of hole.
It using aperture ratio Line Integral analyzer (SA 3100), is calculated according to BET method, activated carbon fiber obtained by the present embodiment
Specific surface area be 1230.96m2/ g, pore-size distribution is as shown in figure 3, activated carbon fiber hole made from as can be seen from the figure
Diameter distribution is concentrated.
Further, absorption property is carried out to activated carbon fiber obtained by the present embodiment and Repeatability is tested, specifically: 1, suction
Attached performance test:
At room temperature, test activated carbon fiber is to Congo red absorption property.Wherein, the concentration of Congo red solution is 200mg/
L, the input amount of activated carbon fiber are 1.0g/L, and the pH value of solution is 6.Adsorption curve is as shown in Figure 4, it is seen that resulting activated carbon
Fibers adsorption effect is strong, function admirable.
2, Repeatability is tested:
The activated carbon fiber of adsorption saturation is washed three times with clear water, tube furnace is put into after drying, is carried out at 800 DEG C high
Temperature regeneration, the activated carbon fiber after test regeneration is at room temperature to Congo red absorption.Wherein, the concentration of Congo red solution is
200mg/L, the input amount of activated carbon fiber are 1.0g/L, and the pH value of solution is 6, and adsorption time 180min is repeated 5 times.This
Influence of the activated carbon fiber regeneration number to adsorption effect made from embodiment the results are shown in Table 1, it is seen that resulting activated carbon fiber
Can multiple recycling and reusing, and good adsorption performance.
Table 1
Embodiment 2
The preparation of activated carbon fiber, the specific steps are as follows:
Cotton linter is immersed in 5% ammonium dihydrogen phosphate, drying is taken out after 1h；Then by the cotton linter after drying
It is put into tube furnace, under the protection of nitrogen, first carries out carbonization-activation, 425 DEG C of carbonization 60min；Then with the speed of 10 DEG C/min
Rate is warming up to 900 DEG C, is passed through steam activation 40min；It is taken out after product natural cooling, is put into vacuum oven, in 60 DEG C
Dry 12h, obtains activated carbon fiber.
It using aperture ratio Line Integral analyzer (SA 3100), is calculated according to BET method, activated carbon fiber obtained by the present embodiment
Specific surface area be 1512.05m2/g。
Embodiment 3
The preparation of activated carbon fiber, the specific steps are as follows:
Cotton linter is immersed in 5% potassium dihydrogen phosphate, drying is taken out after 1h；Then by the cotton linter after drying
It is put into tube furnace, under the protection of nitrogen, first carries out carbonization-activation, 425 DEG C of carbonization 60min；Then with the speed of 10 DEG C/min
Rate is warming up to 900 DEG C, is passed through steam activation 50min；It is taken out after product natural cooling, is put into vacuum oven, in 60 DEG C
Dry 12h, obtains activated carbon fiber.
It using aperture ratio Line Integral analyzer (SA 3100), is calculated according to BET method, activated carbon fiber obtained by the present embodiment
Specific surface area be 1524.09m2/g。
Claims (9)
1. a kind of preparation method of activated carbon fiber, which comprises the following steps:
(1) cotton linter is immersed in phosphate solution after a period of time, takes out drying；
(2) under nitrogen protection, the cotton linter of drying is carbonized, the intermediate after must being carbonized；
(3) continue under nitrogen protection, to be warming up to certain temperature, be passed through vapor, activate the intermediate after carbonization, to
It is dried after product is cooling, obtains activated carbon fibre.
2. the preparation method of activated carbon fiber according to claim 1, which is characterized in that dipping described in step (1)
Time is 60~180min.
3. the preparation method of activated carbon fiber according to claim 1, which is characterized in that phosphate described in step (1)
Solution is one of ammonium hydrogen phosphate, ammonium dihydrogen phosphate, potassium hydrogen phosphate, dibastic sodium phosphate, potassium dihydrogen phosphate, sodium dihydrogen phosphate or several
Kind.
4. the preparation method of activated carbon fiber according to claim 1, which is characterized in that phosphate described in step (1)
The concentration of solution is 1%~10%.
5. the preparation method of activated carbon fiber according to claim 1, which is characterized in that drying described in step (1)
Temperature is 30~60 DEG C.
6. the preparation method of activated carbon fiber according to claim 1, which is characterized in that carbonization described in step (2)
Temperature is 425 DEG C, and the time is 30~120min.
7. the preparation method of activated carbon fiber according to claim 1, which is characterized in that heating described in step (3)
Rate is 6~12 DEG C/min.
8. the preparation method of activated carbon fiber according to claim 1, which is characterized in that certain temperature described in step (3)
Degree is 700~1000 DEG C, and the time of the activation is 30~150min.
9. the preparation method of activated carbon fiber according to claim 1, which is characterized in that dry tool described in step (3)
Body are as follows: under the conditions of 60 DEG C, be dried in vacuo 12h.
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| CN201910221998.0A CN109972235A (en) | 2019-03-22 | 2019-03-22 | A kind of preparation method of activated carbon fiber |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910221998.0A CN109972235A (en) | 2019-03-22 | 2019-03-22 | A kind of preparation method of activated carbon fiber |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114130358A (en) * | 2021-12-06 | 2022-03-04 | 北京碧水源膜科技有限公司 | Activated carbon fiber for efficiently adsorbing smelly substances, filter element prepared from activated carbon fiber and application of activated carbon fiber |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102220665A (en) * | 2011-04-25 | 2011-10-19 | 山东大学 | Method for preparing activated carbon fibers with high specific surface by use of cotton linters |
| CN106040172A (en) * | 2016-06-15 | 2016-10-26 | 绍兴县福兴纺织服饰有限公司 | Preparation method of viscose-based activated carbon fiber cloth |
-
2019
- 2019-03-22 CN CN201910221998.0A patent/CN109972235A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102220665A (en) * | 2011-04-25 | 2011-10-19 | 山东大学 | Method for preparing activated carbon fibers with high specific surface by use of cotton linters |
| CN106040172A (en) * | 2016-06-15 | 2016-10-26 | 绍兴县福兴纺织服饰有限公司 | Preparation method of viscose-based activated carbon fiber cloth |
Non-Patent Citations (1)
| Title |
|---|
| 朱艳云 等: "活性碳纤维对刚果红的吸附及再生研究", 《化学与生物工程》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114130358A (en) * | 2021-12-06 | 2022-03-04 | 北京碧水源膜科技有限公司 | Activated carbon fiber for efficiently adsorbing smelly substances, filter element prepared from activated carbon fiber and application of activated carbon fiber |
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