CN106676677A - Method for preparing hollow carbon fiber from biomass material - Google Patents
Method for preparing hollow carbon fiber from biomass material Download PDFInfo
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- CN106676677A CN106676677A CN201710065135.XA CN201710065135A CN106676677A CN 106676677 A CN106676677 A CN 106676677A CN 201710065135 A CN201710065135 A CN 201710065135A CN 106676677 A CN106676677 A CN 106676677A
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- carbon fiber
- hollow carbon
- deionized water
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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
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
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Abstract
The invention discloses a method for preparing a hollow carbon fiber from a biomass material. The method comprises the following steps: (1) weighing a certain amount of potassium hydroxide, adding into deionized water, and sufficiently stirring until completely dissolving to obtain a solution; (2) adding palm fibers into the solution, putting into a reaction kettle, and performing hydrothermal treatment; (3) after the hydrothermal treatment is completed, taking out the solution, cooling, then pouring the supernatant liquid to leave the product, cleaning the product with deionized water, and performing ultrasonic treatment; (4) transferring the cleaned product into a carbonization furnace, performing heating carbonization treatment in an inert gas protective atmosphere, and then naturally cooling to room temperature; and (5) taking out the carbonized product, treating with an alkaline solution to remove impurities in the material, cleaning with deionized water, then putting into a drying oven, and drying to obtain the hollow carbon fiber. According to the invention, the carbon fiber having a hollow structure can be prepared at high yield; the preparation process is simple, easy to operate and low in cost; and a hollow carbon fiber sample prepared by the preparation method is uniform in size and high in crystallinity.
Description
Technical field
The invention belongs to technical field of carbon fiber preparation, specifically a kind of biological material prepares the side of hollow carbon fiber
Method.
Background technology
Carbon fiber is fibrous carbon materials, containing substantial amounts of carbon.It is high in noble gases using organic fiber
Temperature is carbonized and obtains.Carbon fiber has multiple beneficial performance, such as low-density, good mechanical property, absorption property.Carbon fiber
The every field in military and civilian industry obtains extensive application.Therefore the concern of various countries researcher is caused.However, carbon
The carbon fiber that fiber product is mainly prepared by petrochemical materials is processed, complex process, cost intensive, and fossil energy
Source increasingly depleted.
The content of the invention
Goal of the invention：In order to overcome the deficiencies in the prior art, the present invention to provide in a kind of biological material preparation
The method of empty carbon fiber.
Technical scheme：To solve above-mentioned technical problem, a kind of biological material of the present invention prepares the side of hollow carbon fiber
Method, comprises the following steps：(1) weigh a certain amount of potassium hydroxide, add to be stirred well to be completely dissolved in deionized water and obtain
Solution；(2) after Petiolus Trachycarpi silk is added in the solution of step (1), being put in reactor carries out hydrothermal treatment consists；(3) hydrothermal treatment consists are complete
Take out after finishing and solution and cool down, supernatant liquid is poured out after cooling and product is left, deionized water wash products and supersound process；
(4) product obtained after cleaning is proceeded in retort, carbonization treatment is heated under inert gas shielding, natural cooling after carbonization
To room temperature；(5) product of carbonization treatment is taken out, impurity in material is removed using alkaline solution process, after deionized water cleaning
Insert oven for drying (being originally used for baking), you can obtain hollow carbon fiber.
Wherein, deionized water and potassium hydroxide, the mass percent of Petiolus Trachycarpi silk are 76~80:17.5~21:2.5~3.5.
Wherein, the temperature of reactor is set as 160 DEG C -180 DEG C, and hydrothermal conditions are 8-10h.
Wherein, the product obtained after cleaning is proceeded in retort and is uniformly added with 1 DEG C/min programming rates under noble gases
Heat is to 700-1000 DEG C of carbonization treatment, carbonization treatment 2-5h.
Wherein, insert 60 DEG C of baking oven after deionized water cleaning and be dried 12h.
Wherein, sonication treatment time is 5min.
Wherein, the alkaline solution in step (5) is 3M NaOH solutions.
Beneficial effect：The method that a kind of biological material of the present invention prepares hollow carbon fiber, has the advantages that：
1) present invention is obtained in that the carbon fiber with hollow structure of high yield；
2) preparation process is simple, easily operated, low cost of the invention；
3) present invention need not prepare hollow carbon fiber using petrochemical industry material；
4) hollow carbon fiber sample size is uniform obtained in preparation method of the invention, and degree of crystallinity is high, good conductivity.
Description of the drawings
Fig. 1 is the XRD spectrum of hollow carbon fiber obtained in the embodiment of the present invention 1；
Fig. 2 is the Raman picture of raw material Petiolus Trachycarpi silk obtained in the embodiment of the present invention 1；
Fig. 3 a are the low power SEM picture of the raw material Petiolus Trachycarpi silk in the present invention；
Fig. 3 b are times SEM pictures in Petiolus Trachycarpi silk in the present invention after hydrothermal treatment consists；
Fig. 3 c are the Petiolus Trachycarpi silk high power SEM picture in the present invention after hydrothermal treatment consists；
Fig. 4 a are the SEM pictures of hollow carbon fiber prepared by the present invention；
Fig. 4 b are the SEM pictures of hollow carbon fiber prepared by the present invention；
Fig. 5 is the Raman picture of raw material Petiolus Trachycarpi silk obtained in the embodiment of the present invention 4；
Fig. 6 is the Raman picture of raw material Petiolus Trachycarpi silk obtained in the embodiment of the present invention 5.
Specific embodiment
The present invention is further described with reference to embodiment.
Embodiment 1
Mesoporous carbon fiber is prepared using simple hydro-thermal reaction using wood material in the present embodiment.Preparation method：First measure
60ml deionized waters are taken, then weighs potassium hydroxide 16g, be stirred well to and be completely dissolved, it is then again that Petiolus Trachycarpi silk 2g additions is above-mentioned
Solution, in being subsequently adding the reactor of 100ml.Proceeding to 160 degree of baking oven carries out hydrothermal treatment consists 8h, and upper liquid is poured out after cooling, uses
Deionized water wash products and supersound process.Hydrothermal product is proceeded in retort under noble gases with 1 DEG C/min programming rates
It is uniformly heated to 700 DEG C.Room temperature is naturally cooled to after carbonization 2h.Product is taken out, is removed in material using the process of 3M NaOH solutions
Impurity.The night of baking oven one is inserted after deionized water cleaning, you can obtain hollow carbon fiber.
The XRD spectrum of the hollow carbon fiber that the present embodiment is prepared is as shown in Figure 1, it is seen that the mesoporous carbon for preparing is fine
The degree of crystallinity of dimension is very high, without dephasign.The Raman figure of hollow carbon fiber is as shown in Fig. 2 the hollow carbon after high-temperature process is fine
G peaks and D peaks are occurred in that in dimension Raman spectrum.The SEM figures of product after raw material and hydrothermal treatment consists, as shown in figure 3, product after hydro-thermal
In threadiness and be interweaved together.Shown in SEM Fig. 4 of hollow carbon fiber, wherein comprising two width figures, respectively making
The SEM pictures of the standby hollow carbon fiber different piece for obtaining, it can be seen that the diameter of prepared hollow carbon fiber exists
Between 1-5 μm, in Fig. 4 (b), hence it is evident that see tubular structure.
Embodiment 2
Mesoporous carbon fiber is prepared using simple hydro-thermal reaction using wood material in the present embodiment.Preparation method：First measure
80ml deionized waters are taken, then weighs potassium hydroxide 18g, be stirred well to and be completely dissolved, it is then again that Petiolus Trachycarpi silk 3g additions is above-mentioned
Solution, in being subsequently adding the reactor of 100ml.Proceeding to 160 DEG C of baking oven carries out hydrothermal treatment consists 10h, and upper liquid is poured out after cooling, uses
Deionized water wash products and supersound process.Hydrothermal product is proceeded in retort under noble gases with 1 DEG C/min programming rates
It is uniformly heated to 1000 DEG C.Room temperature is naturally cooled to after carbonization 2h.Product is taken out, is removed using 3M NaOH process miscellaneous in material
Matter.The night of baking oven one is inserted after deionized water cleaning, you can obtain hollow carbon fiber.
The XRD spectrum of the hollow carbon fiber that embodiment is prepared is as shown in Figure 1, it is seen that the mesoporous carbon for preparing is fine
The degree of crystallinity of dimension is very high, without dephasign.The Raman figure of hollow carbon fiber is as shown in figure 5, the hollow carbon after high-temperature process is fine
G peaks and D peaks are occurred in that in dimension Raman spectrum.The SEM figures of product after raw material and hydrothermal treatment consists, as shown in figure 3, product after hydro-thermal
In threadiness and be interweaved together.Shown in SEM Fig. 4 of hollow carbon fiber, wherein comprising two width figures, respectively making
The SEM pictures of the standby hollow carbon fiber different piece for obtaining, it can be seen that the diameter of prepared hollow carbon fiber exists
Between 1-5 μm, in Fig. 4 (b), hence it is evident that see tubular structure.
Embodiment 3
Mesoporous carbon fiber is prepared using simple hydro-thermal reaction using wood material in the present embodiment.Preparation method：First measure
80ml deionized waters are taken, then weighs potassium hydroxide 18g, be stirred well to and be completely dissolved, it is then again that Petiolus Trachycarpi silk 3g additions is above-mentioned
Solution, in being subsequently adding the reactor of 100ml.Proceeding to 180 DEG C of baking oven carries out hydrothermal treatment consists 8h, and upper liquid is poured out after cooling, uses
Deionized water wash products and supersound process.Hydrothermal product is proceeded in retort under noble gases with 1 DEG C/min programming rates
It is uniformly heated to 700 DEG C.Room temperature is naturally cooled to after carbonization 5h.Product is taken out, is removed using 3M NaOH process miscellaneous in material
Matter.The night of baking oven one is inserted after deionized water cleaning, you can obtain hollow carbon fiber.
The XRD spectrum of the hollow carbon fiber that embodiment is prepared is as shown in Figure 1, it is seen that the mesoporous carbon for preparing is fine
The degree of crystallinity of dimension is very high, without dephasign.The Raman figure of hollow carbon fiber is as shown in Fig. 2 the hollow carbon after high-temperature process is fine
G peaks and D peaks are occurred in that in dimension Raman spectrum.The SEM figures of product after raw material and hydrothermal treatment consists, as shown in figure 3, product after hydro-thermal
In threadiness and be interweaved together.Shown in SEM Fig. 4 of hollow carbon fiber, wherein comprising two width figures, respectively making
The SEM pictures of the standby hollow carbon fiber different piece for obtaining, it can be seen that the diameter of prepared hollow carbon fiber exists
Between 1-5 μm, in Fig. 4 (b), hence it is evident that see tubular structure.
Embodiment 4
Mesoporous carbon fiber is prepared using simple hydro-thermal reaction using wood material in the present embodiment.Preparation method：First measure
80ml deionized waters are taken, then weighs potassium hydroxide 18g, be stirred well to and be completely dissolved, it is then again that Petiolus Trachycarpi silk 3g additions is above-mentioned
Solution, in being subsequently adding the reactor of 100ml.Proceeding to 180 DEG C of baking oven carries out hydrothermal treatment consists 10h, and upper liquid is poured out after cooling, uses
Deionized water wash products and supersound process.Hydrothermal product is proceeded in retort under noble gases with 1 DEG C/min programming rates
It is uniformly heated to 1000 DEG C.Room temperature is naturally cooled to after carbonization 5h.Product is taken out, is removed using 3M NaOH process miscellaneous in material
Matter.The night of baking oven one is inserted after deionized water cleaning, you can obtain hollow carbon fiber.
The XRD spectrum of the hollow carbon fiber that embodiment is prepared is as shown in Figure 1, it is seen that the mesoporous carbon for preparing is fine
The degree of crystallinity of dimension is very high, without dephasign.The Raman figure of hollow carbon fiber is as shown in figure 5, the hollow carbon after high-temperature process is fine
G peaks and D peaks are occurred in that in dimension Raman spectrum.The SEM figures of product after raw material and hydrothermal treatment consists, as shown in figure 3, product after hydro-thermal
In threadiness and be interweaved together.Shown in SEM Fig. 4 of hollow carbon fiber, wherein comprising two width figures, respectively making
The SEM pictures of the standby hollow carbon fiber different piece for obtaining, it can be seen that the diameter of prepared hollow carbon fiber exists
Between 1-5 μm, in Fig. 4 (b), hence it is evident that see tubular structure.
Embodiment 5
Mesoporous carbon fiber is prepared using simple hydro-thermal reaction using wood material in the present embodiment.Preparation method：First measure
70ml deionized waters are taken, then weighs potassium hydroxide 17g, be stirred well to and be completely dissolved, it is then again that Petiolus Trachycarpi silk 3g additions is above-mentioned
Solution, in being subsequently adding the reactor of 100ml.Proceeding to 170 DEG C of baking oven carries out hydrothermal treatment consists 9h, and upper liquid is poured out after cooling, uses
Deionized water wash products and supersound process.Hydrothermal product is proceeded in retort under noble gases with 1 DEG C/min programming rates
It is uniformly heated to 1000 DEG C.Room temperature is naturally cooled to after carbonization 5h.Product is taken out, is removed using 3M NaOH process miscellaneous in material
Matter.The night of baking oven one is inserted after deionized water cleaning, you can obtain hollow carbon fiber.
The XRD spectrum of the hollow carbon fiber that embodiment is prepared is as shown in Figure 1, it is seen that the mesoporous carbon for preparing is fine
The degree of crystallinity of dimension is very high, without dephasign.The Raman figure of hollow carbon fiber is as shown in fig. 6, the hollow carbon after high-temperature process is fine
G peaks and D peaks are occurred in that in dimension Raman spectrum.The SEM figures of product after raw material and hydrothermal treatment consists, as shown in figure 3, product after hydro-thermal
In threadiness and be interweaved together.Shown in SEM Fig. 4 of hollow carbon fiber, wherein comprising two width figures, respectively making
The SEM pictures of the standby hollow carbon fiber different piece for obtaining, it can be seen that the diameter of prepared hollow carbon fiber exists
Between 1-5 μm, in Fig. 4 (b), hence it is evident that see tubular structure.
The above is only the preferred embodiment of the present invention, it should be pointed out that：For the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (7)
1. a kind of method that biological material prepares hollow carbon fiber, it is characterised in that comprise the following steps：(1) weigh certain
The potassium hydroxide of amount, adds and is stirred well to be completely dissolved and obtains solution in deionized water；(2) Petiolus Trachycarpi silk is added into step (1)
Solution in after, being put in reactor carries out hydrothermal treatment consists；(3) solution is taken out after hydrothermal treatment consists are finished and is cooled down, fallen after cooling
Go out supernatant liquid and leave product, deionized water wash products and supersound process；(4) product obtained after cleaning is proceeded to into charcoal
In changing stove, carbonization treatment is heated under inert gas shielding, room temperature is naturally cooled to after carbonization；(5) product of carbonization treatment is taken out
Thing, removes impurity in material, after baking oven baking is inserted after deionized water cleaning, you can obtain hollow using alkaline solution process
Carbon fiber.
2. the method that a kind of biological material according to claim 1 prepares hollow carbon fiber, it is characterised in that：Wherein,
Deionized water and potassium hydroxide, the mass percent of Petiolus Trachycarpi silk are 76~80:17.5~21:2.5~3.5.
3. the method that a kind of biological material according to claim 1 prepares hollow carbon fiber, it is characterised in that：Wherein,
The temperature of reactor is set as 160 DEG C -180 DEG C, and hydrothermal conditions are 8-10h.
4. the method that a kind of biological material according to claim 1 prepares hollow carbon fiber, it is characterised in that：Wherein,
The product obtained after cleaning is proceeded in retort and is uniformly heated to 700-1000 DEG C with 1 DEG C/min programming rates under noble gases
Carbonization treatment, carbonization treatment 2-5h.
5. the method that a kind of biological material according to claim 1 prepares hollow carbon fiber, it is characterised in that：Wherein,
Baking oven is inserted after deionized water cleaning be dried 12h at a temperature of 60 DEG C.
6. the method that a kind of biological material according to claim 1 prepares hollow carbon fiber, it is characterised in that：Wherein,
Sonication treatment time is 5min.
7. the method that a kind of biological material according to claim 1 prepares hollow carbon fiber, it is characterised in that：Wherein,
Alkaline solution in step (5) is 3M NaOH solutions.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107177905A (en) * | 2017-06-26 | 2017-09-19 | 河南工程学院 | A kind of carbon fiber prepared based on discarded bamboo chopsticks hydrothermal carbonization method and its application |
| CN109004199A (en) * | 2018-08-01 | 2018-12-14 | 北京理工大学 | A kind of preparation method of sodium-ion battery cathode biomass hard carbon material |
| CN109371505A (en) * | 2018-09-27 | 2019-02-22 | 安徽工程大学 | A kind of biomass-based screw carbon fibre and preparation method thereof |
| CN109759101A (en) * | 2019-03-27 | 2019-05-17 | 合肥学院 | A kind of method that wood fiber biomass prepares carbon carried heteropoly acid material |
| CN114737279A (en) * | 2022-03-25 | 2022-07-12 | 北京科技大学 | Biomass hollow carbon fiber, preparation method thereof, electrode material and battery |
| CN117117179A (en) * | 2023-10-25 | 2023-11-24 | 浙江帕瓦新能源股份有限公司 | Carbon negative electrode material, preparation method thereof and sodium ion battery |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107177905A (en) * | 2017-06-26 | 2017-09-19 | 河南工程学院 | A kind of carbon fiber prepared based on discarded bamboo chopsticks hydrothermal carbonization method and its application |
| CN109004199A (en) * | 2018-08-01 | 2018-12-14 | 北京理工大学 | A kind of preparation method of sodium-ion battery cathode biomass hard carbon material |
| CN109371505A (en) * | 2018-09-27 | 2019-02-22 | 安徽工程大学 | A kind of biomass-based screw carbon fibre and preparation method thereof |
| CN109371505B (en) * | 2018-09-27 | 2021-03-02 | 安徽工程大学 | Biomass-based spiral carbon fiber and preparation method thereof |
| CN109759101A (en) * | 2019-03-27 | 2019-05-17 | 合肥学院 | A kind of method that wood fiber biomass prepares carbon carried heteropoly acid material |
| CN114737279A (en) * | 2022-03-25 | 2022-07-12 | 北京科技大学 | Biomass hollow carbon fiber, preparation method thereof, electrode material and battery |
| CN114737279B (en) * | 2022-03-25 | 2023-02-24 | 北京科技大学 | Biomass hollow carbon fiber, preparation method thereof, electrode material and battery |
| CN117117179A (en) * | 2023-10-25 | 2023-11-24 | 浙江帕瓦新能源股份有限公司 | Carbon negative electrode material, preparation method thereof and sodium ion battery |
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Application publication date: 20170517 |