CN103397404A - Method for increasing specific surface area of wooden active carbon fiber - Google Patents
Method for increasing specific surface area of wooden active carbon fiber Download PDFInfo
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Abstract
The invention provides a method for increasing the specific surface area of a wooden active carbon fiber. The method comprises the following process steps of: carrying out pre-oxidation treatment on a wooden active carbon fiber precursor, and activating the obtained pre-oxidized fiber so as to obtain the wooden active carbon fiber. Compared with the wooden active carbon fiber which is not subjected to the pre-oxidation treatment, the wooden active carbon fiber prepared by utilizing the method has the advantage that the specific surface area is greatly increased; and the method is convenient to operate, is low in energy consumption and has a relatively good industrial application prospect.
Description
Technical field
The present invention relates to the chemical fibre field, particularly, relate to a kind of by pre-oxidation treatment, thereby wooden activated carbon fiber that specific area is improved and preparation method thereof.
Background technology
Activated carbon fiber (Activated Carbon Fiber; be called for short ACF) be a kind of new sorbing material that rises at present; as a kind of Novel adsorption functional material; can be widely used in the aspects such as the depollution of environment, catalyst carrier, electrode material; compare with active carbon; it possesses the characteristics such as diameter is thin, specific area is high, adsorption capacity is large, adsorption desorption speed is fast, is described as one of state-of-the-art environmental protection material of 21 century.At present, the raw materials of activated carbon fiber is mainly take petrochemicals as main,, although the product of preparing has good absorption property,, because petroleum resources are day by day in short supply, makes activated carbon fiber not have sustainable developability.In the today of highly advocating energy greenization, how preparing the activated carbon fiber of wooden activated carbon fiber replacement take the petrochemical industry resource as raw material becomes an important topic.
At present, the core technology of activated carbon fiber mainly rest in external monopoly enterprise especially Japan, in U.S.'s hand, developed the different material base, had the extraordinary activated carbon fiber product of different absorption properties.Activated carbon fiber and products thereof is in developed countries such as Japan, the U.S., industrialization and practical stage have been entered, and the activated carbon fiber of China also is in development, exploitation and experimental stage basically, not yet can start the kind with industrialization value, properties of product need further raising.
The Wooden Biomass resource is renewable, and it contains enriches cellulose and lignin is all the good precursor raw materials that prepare activated carbon fiber, and a large amount of discarded timber and wood machining residues all can become the raw material sources of activated carbon fiber.Utilize the precursor material of the biomass resource such as timber as activated carbon fiber, can realize the sustainable use of activated carbon fiber raw material, reduce the production cost of activated carbon fiber, at aspects such as environmental protection and resources reserves, have great strategic importance.
Current, in the world,, in order to improve the specific area of wooden activated carbon fiber, improve its characterization of adsorption, general by changing the means of activation parameter, as improving activation temperature, the prolongation soak time, strengthen activator concentration etc.But the complex operation of these methods,, due to the higher activation temperature of needs, cause power consumption large, is not suitable with the requirement of conservation-minded society.Therefore in the urgent need to a kind of method of the easy to operate and wooden activated carbon fiber specific area of raising that energy consumption is low.
Summary of the invention
The object of the present invention is to provide a kind of method that improves wooden activated carbon fiber specific area.
The wooden activated carbon fiber that provides a kind of specific area high is provided.
A kind of method that improves wooden activated carbon fiber specific area provided by the invention comprises the following steps:
(1) timber liquefied matter, through synthetic, melt spinning and the curing process of spinning solution, makes the timber liquefied matter precursor, and precursor, by pre-oxidation treatment, is prepared preoxided thread;
(2) preoxided thread is made activation processing, obtain wooden activated carbon fiber.
By well known to a person skilled in the art technological means, timber liquefied matter makes the timber liquefied matter precursor through synthetic, melt spinning and the curing process of spinning solution, and the method is open in Chinese patent CN102719935A.
Wherein, the pre-oxidation treatment of step (1) is that precursor is put into pre-oxidation furnace, and the precursor two ends are fixed, and pass into air, and air mass flow is 0.2-0.6m
3/ h, first heat up, then lower the temperature, and stops passing into air, takes out preoxided thread
In above-mentioned steps (1), heating rate is 0.5-1 ℃/min, is warming up to 200-280 ℃, is down to room temperature after insulation 40-80min, stops passing into air, takes out preoxided thread.
Wherein, to put into the quality of the precursor of pre-oxidation furnace be 1-2g to step (1).
Preferably, air mass flow is 0.6m
3/ h, heating rate are 1 ℃/min.
Preferably, the quality of putting into the pre-oxidation furnace precursor is 1.5g.
In described step (1), be heated to be down to room temperature after 280 ℃ of insulation 60min, stop passing into air, take out preoxided thread.
In the step of the inventive method (2), the activation processing step is as follows:
Under inert gas or nitrogen protection, preoxided thread is made activation processing, activation temperature is 650-910 ℃, and the activator that uses is water vapour, and steam rates is 3.9～7.1g/min, and soak time is 30-60min, obtains wooden activated carbon fiber.
Preferably, in the activation processing step, steam rates is 4.84g/min, and soak time is 60min.
The wooden activated carbon fiber that the inventive method prepares is also in protection scope of the present invention.
The present invention improves the method for wooden activated carbon fiber, and in step (1), the technological parameter of pre-oxidation step is as follows:
The 1-2g precursor is put into pre-oxidation furnace, and two ends are fixed with clip, open the air generating pump and pass into a certain amount of air, and air mass flow is 0.2-0.6m
3/ h, heating rate is 0.5-1 ℃/min, is heated to be down to room temperature after 200-280 ℃ of insulation 40-80min, closes the air generating pump, takes out preoxided thread.
Pass through great many of experiments, in conjunction with its result, the inventor finds in step (1), not only the selection of Pre oxidation scope is a key factor, simultaneously, the quality of precursor, air velocity and heating rate also have larger impact to oxidizing process, if temperature is not enough, precursor adds too much, heating rate is excessively slow, the products therefrom degree of oxidation is obviously not enough, and the sorption and desorption ability is poor, and specific area is little, vice versa, the wooden activated carbon fiber quality of gained obviously descends, and can't reach technologic requirement, more can't meet the large-scale production demand.In the condition and range of pre-oxidation of the present invention, can realize extraordinary effect.
For the technological parameter of the step (2) of the inventive method, specific as follows:
Under nitrogen protection, preoxided thread is made activation processing, activation temperature is 650-910 ℃, and the activator that uses is water vapour, and flow is 3.9-7.1g/min, and soak time is 30-60min, obtains wooden activated carbon fiber.
Preferably, the wooden activated carbon fiber specific area of raising of the present invention method is:
1) preparation of pre-oxygen silk: timber liquefied matter is through synthetic, melt spinning and the curing process of spinning solution, make the timber liquefied matter precursor, then the 1.5g precursor is put into pre-oxidation furnace, two ends are fixed with clip, open the air generating pump and pass into a certain amount of air, air mass flow is 0.6m
3/ h, heating rate is 1 ℃/min, is heated to be down to room temperature after 280 ℃ of insulation 60min, closes the air generating pump, takes out preoxided thread.
2) under nitrogen protection, preoxided thread is made activation processing; activation temperature is that 910 ℃ of activators that use are water vapour, and flow is 4.84g/min, and soak time is 60min; obtain the wooden activated carbon fiber of function admirable, the specific area of the wooden activated carbon fiber of gained has reached 3068m
2/ g, total pore volume has reached 1.728cc/g.
The wooden activated carbon fiber that the inventive method obtains has larger specific area, and,, owing to being fibrous, can being woven into the various ways such as cloth, band, felt and using, for the engineering application provides certain flexibility, thereby solved the insurmountable problem of many granular active carbons.
In addition, by special processing mode of the present invention, at first carry out pre-oxidation, then activate, make the wooden activated carbon fiber of gained possess excellent physicochemical property, specific area increases greatly, and the adsorption and desorption ability all is improved, and with its special surface chemical structure and physical adsorption characteristic, is widely used in the fields such as environmental protection, electronics, medical sanitary, chemical industry.And method of the present invention is easy to operate, and energy consumption is little, has prospects for commercial application preferably.
Description of drawings
Fig. 1 is the pre-oxidation treatment group of embodiment 1 and the nitrogen adsorption of control group-desorption curve comparison figure.Wherein, relative pressure is the ratio of the saturated vapor pressure of nitrogen under nitrogen partial pressure and liquid nitrogen temperature.
Fig. 2 is the pre-oxidation treatment group of embodiment 2 and the nitrogen adsorption of control group-desorption curve comparison figure.
Fig. 3 is the pre-oxidation treatment group of embodiment 3 and the nitrogen adsorption of control group-desorption curve comparison figure.
Fig. 4 is the pre-oxidation treatment group of embodiment 4 and the nitrogen adsorption of control group-desorption curve comparison figure.
Fig. 5 is the pre-oxidation treatment group of embodiment 5 and the nitrogen adsorption of control group-desorption curve comparison figure.
Fig. 6 is the pre-oxidation treatment group of embodiment 6 and the nitrogen adsorption of control group-desorption curve comparison figure.
The specific embodiment
Following examples further illustrate content of the present invention, but should not be construed as limitation of the present invention.Without departing from the spirit and substance of the case in the present invention, modification or replacement to the inventive method, step or condition are done, all belong to scope of the present invention.
If do not specialize, the conventional means that in embodiment, technological means used is well known to those skilled in the art, in embodiment, each raw material that adds except specifying, is commercially available conventional raw material.
Embodiment 1 improves the method (1) of wooden activated carbon fiber
Timber liquefied matter is through synthetic, melt spinning and the curing process of spinning solution, make timber liquefied matter precursor (method is referring to Chinese patent CN102719935A), then the 1.5g precursor is put into pre-oxidation furnace, two ends are fixed with clip, and opening the air generating pump, to pass into flow be 0.6m
3The air of/h, heating rate is 1 ℃/min, is heated to be down to room temperature after 200 ℃ of insulation 60min, closes the air generating pump, takes out preoxided thread.Repeat above step and make the pre-oxygen silk of 5g, then it is carried out under 650 ℃ activation processing under nitrogen protection, the activator that uses is steam, and flow is 4.84g/min, and soak time is 60min, obtains wooden activated carbon fiber.Establish simultaneously control group, be the group that directly precursor is activated without pre-oxidation treatment, each parameter of its activation step is with the pre-oxidation treatment group.
According to the nitrogen adsorption desorption curve map that the Autosorb-iQ nitrogen adsorption instrument that adopts Quantachrome instrument company to provide obtains, the specific area that adopts multiple spot BET method to survey the wooden activated carbon fiber of institute's the present embodiment acquisition is 701m
2/ g, than the wooden activated carbon fiber specific area 665m of control group (without pre-oxidation treatment)
2/ g has increased by 5.4%, sees Fig. 1.Adopt nitrogen capacity corresponding to nitrogen adsorption curve relative pressure peak to record total pore volume and reached 0.385/g, total pore volume 0.373cc/g has increased by 3.2% than the wooden activated carbon fiber of control group (without pre-oxidation treatment).
Embodiment 2 improves the method (2) of wooden activated carbon fiber
Timber liquefied matter, through synthetic, melt spinning and the curing process of spinning solution, makes the timber liquefied matter precursor, then the 1.5g precursor is put into pre-oxidation furnace, and two ends are fixed with clip, and opening the air generating pump, to pass into flow be 0.6m
3The air of/h, heating rate is 1 ℃/min, is heated to be down to room temperature after 280 ℃ of insulation 60min, closes the air generating pump, takes out preoxided thread.Repeat above step and make the pre-oxygen silk of 5g, then it is carried out under 650 ℃ activation processing under nitrogen protection, the activator that uses is steam, and flow is 4.84g/min, and soak time is 40min, obtains wooden activated carbon fiber.Establish simultaneously control group, be the group that directly precursor is activated without pre-oxidation treatment, each parameter of its activation step is with the pre-oxidation treatment group.
According to the nitrogen adsorption desorption curve map that the Autosorb-iQ nitrogen adsorption instrument that adopts Quantachrome instrument company to provide obtains, the specific area of the wooden activated carbon fiber that the present embodiment that adopts multiple spot BET method to record obtains is 779m
2/ g, than the wooden activated carbon fiber specific area 665m of control group (without pre-oxidation treatment)
2/ g has increased by 17.1%, sees Fig. 2.Adopt nitrogen capacity corresponding to nitrogen adsorption curve relative pressure peak to record total pore volume and reached 0.480cc/g, total pore volume 0.373cc/g has increased by 28.7% than the wooden activated carbon fiber of control group (without pre-oxidation treatment).
Embodiment 3 improves the method (3) of wooden activated carbon fiber
Timber liquefied matter, through synthetic, melt spinning and the curing process of spinning solution, makes the timber liquefied matter precursor, then the 1g precursor is put into pre-oxidation furnace, and two ends are fixed with clip, and opening the air generating pump, to pass into flow be 0.2m
3The air of/h, heating rate is 0.5 ℃/min, is heated to be down to room temperature after 240 ℃ of insulation 40min, closes the air generating pump, takes out preoxided thread.Repeat above step and make the pre-oxygen silk of 4.5g, then it is carried out under 800 ℃ activation processing under nitrogen protection, the activator that uses is steam, and flow is 7.1g/min, and soak time is 30min, obtains wooden activated carbon fiber.Establish simultaneously control group, be the group that directly precursor is activated without pre-oxidation treatment, each parameter of its activation step is with the pre-oxidation treatment group.
According to the nitrogen adsorption desorption curve map that the Autosorb-iQ nitrogen adsorption instrument that adopts Quantachrome instrument company to provide obtains, the specific area of the wooden activated carbon fiber of the present embodiment that employing multiple spot BET method records is 969m
2/ g, than the wooden activated carbon fiber specific area 871m of control group (without pre-oxidation treatment)
2/ g has increased by 11.3%, sees Fig. 3.Adopt nitrogen capacity corresponding to nitrogen adsorption curve relative pressure peak to record total pore volume and reached 0.453cc/g, total pore volume 0.434cc/g has increased by 4.4% than the wooden activated carbon fiber of control group (without pre-oxidation treatment).
Embodiment 4 improves the method (4) of wooden activated carbon fiber
Timber liquefied matter, through synthetic, melt spinning and the curing process of spinning solution, makes the timber liquefied matter precursor, then the 2g precursor is put into pre-oxidation furnace, and two ends are fixed with clip, and opening the air generating pump, to pass into flow be 0.6m
3The air of/h, heating rate is 1 ℃/min, is heated to be down to room temperature after 240 ℃ of insulation 60min, closes the air generating pump, takes out preoxided thread.Repeat above step and make the pre-oxygen silk of 5g, then it is carried out activation processing under 910 ℃ under the helium protection, the activator that uses is steam, and flow is 4.84g/min, and soak time is 60min, obtains wooden activated carbon fiber.Establish simultaneously control group, be the group that directly precursor is activated without pre-oxidation treatment, each parameter of its activation step is with the pre-oxidation treatment group.
, according to the nitrogen adsorption desorption curve map that the Autosorb-iQ nitrogen adsorption instrument that adopts Quantachrome instrument company to provide obtains, adopt multiple spot BET method method to be measured as 2877m to the specific area of the wooden activated carbon fiber of gained
2/ g, than the wooden activated carbon fiber specific area 2592m of control group (without pre-oxidation treatment)
2/ g has increased by 11.0%, sees Fig. 4.Adopt nitrogen capacity corresponding to nitrogen adsorption curve relative pressure peak to record total pore volume and reached 1.476cc/g, total pore volume 1.313cc/g has increased by 12.4% than the wooden activated carbon fiber of control group (without pre-oxidation treatment).
Embodiment 5 improves the method (5) of wooden activated carbon fiber
Timber liquefied matter, through synthetic, melt spinning and the curing process of spinning solution, makes the timber liquefied matter precursor, then the 1.5g precursor is put into pre-oxidation furnace, and two ends are fixed with clip, and opening the air generating pump, to pass into flow be 0.6m
3The air of/h, heating rate is 1 ℃/min, is heated to be down to room temperature after 280 ℃ of insulation 60min, closes the air generating pump, takes out preoxided thread.Repeat above step and make the pre-oxygen silk of 4g, then it is carried out activation processing under 910 ℃ under the helium protection, the activator that uses is steam, and flow is 4.84g/min, and soak time is 60min, obtains wooden activated carbon fiber.Establish simultaneously control group, be the group that directly precursor is activated without pre-oxidation treatment, each parameter of its activation step is with the pre-oxidation treatment group.
According to the nitrogen adsorption desorption curve map that the Autosorb-iQ nitrogen adsorption instrument that adopts Quantachrome instrument company to provide obtains, the specific area that adopts multiple spot BET method to record wooden activated carbon fiber is 3068m
2/ g, than the wooden activated carbon fiber specific area 2592m of control group (without pre-oxidation treatment)
2/ g has increased by 18.4%, sees Fig. 5.Adopt nitrogen capacity corresponding to nitrogen adsorption curve relative pressure peak to record total pore volume and reached 1.728cc/g, total pore volume 1.313cc/g has increased by 31.6% than the wooden activated carbon fiber of control group (without pre-oxidation treatment).
Embodiment 6 improves the method (6) of wooden activated carbon fiber
Timber liquefied matter is through synthetic, melt spinning and the curing process of spinning solution, make timber liquefied matter precursor (method is referring to Chinese patent CN102719935A), then the 1.5g precursor is put into pre-oxidation furnace, two ends are fixed with clip, and opening the air generating pump, to pass into flow be 0.6m
3The air of/h, heating rate is 0.5 ℃/min, is heated to be down to room temperature after 240 ℃ of insulation 60min, closes the air generating pump, takes out preoxided thread.Repeat above step and make the pre-oxygen silk of 4.5g, then it is carried out under 910 ℃ activation processing under nitrogen protection, the activator that uses is steam, and flow is 3.9g/min, and soak time is 50min, obtains wooden activated carbon fiber.Establish simultaneously control group, be the group that directly precursor is activated without pre-oxidation treatment, each parameter of its activation step is with the pre-oxidation treatment group.
According to the nitrogen adsorption desorption curve map that the Autosorb-iQ nitrogen adsorption instrument that adopts Quantachrome instrument company to provide obtains, the specific area that adopts multiple spot BET method to survey the wooden activated carbon fiber of institute's the present embodiment acquisition is 2731m
2/ g, than the wooden activated carbon fiber specific area 2592m of control group (without pre-oxidation treatment)
2/ g has increased by 5.4%, sees Fig. 6.Adopt nitrogen capacity corresponding to nitrogen adsorption curve relative pressure peak to record total pore volume and reached 1.361cc/g, total pore volume 1.313cc/g has increased by 3.7% than the wooden activated carbon fiber of control group (without pre-oxidation treatment).
Claims (10)
1. a method that improves wooden activated carbon fiber specific area, is characterized in that, comprises the following steps:
(1) timber liquefied matter, through synthetic, melt spinning and the curing process of spinning solution, makes the timber liquefied matter precursor, and precursor, by pre-oxidation treatment, is prepared preoxided thread;
(2) preoxided thread is made activation processing, obtain wooden activated carbon fiber.
2. the method for claim 1, is characterized in that, the pre-oxidation treatment of step (1) is that precursor is put into pre-oxidation furnace, and the precursor two ends are fixed, and pass into air, and air mass flow is 0.2-0.6m
3/ h, first heat up, then lower the temperature, and stops passing into air, takes out preoxided thread.
3. method as claimed in claim 2, is characterized in that, heating rate is 0.5-1 ℃/min, is warming up to 200-280 ℃, is down to room temperature after insulation 40-60min, stops passing into air, takes out preoxided thread.
4. method as claimed in claim 2, is characterized in that, the quality of putting into the precursor of pre-oxidation furnace is 1-2g.
5. method as claimed in claim 2, is characterized in that, air mass flow is 0.6m
3/ h, heating rate are 1 ℃/min.
6. method as claimed in claim 2, is characterized in that, it is characterized in that, the quality of putting into the pre-oxidation furnace precursor is 1.5g.
7. method as claimed in claim 2, is characterized in that, in described step (1), is heated to be down to room temperature after 280 ℃ of insulation 60min, stops passing into air, takes out preoxided thread.
8. the method for claim 1, is characterized in that, in described step (2), the activation processing step is as follows:
Under inert gas or nitrogen protection, preoxided thread is made activation processing, activation temperature is 650-910 ℃, and the activator that uses is water vapour, and steam rates is 3.9～7.1g/min, and soak time is 30-60min, obtains wooden activated carbon fiber.
9. method as claimed in claim 8, is characterized in that, steam rates is 4.84g/min, and soak time is 60min.
10. the wooden activated carbon fiber for preparing of the arbitrary described method of claim 1-9.
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| CN104307470A (en) * | 2014-09-30 | 2015-01-28 | 天津理工大学 | Preparation method of cellulose fiber-based active carbon fibers with high adsorption capacity as well as product and application of cellulose fiber-based active carbon fibers with high adsorption capacity |
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| CN106702538A (en) * | 2016-12-08 | 2017-05-24 | 北京化工大学 | Preparation method of high-performance activated carbon fibers |
| CN107934955A (en) * | 2017-11-17 | 2018-04-20 | 浙江大学 | A kind of method of activation process commercialization carbon cloth |
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| CN107934955A (en) * | 2017-11-17 | 2018-04-20 | 浙江大学 | A kind of method of activation process commercialization carbon cloth |
| CN109224627A (en) * | 2018-08-17 | 2019-01-18 | 安徽三联学院 | Atmospheric particulates filtering material |
| CN109680363A (en) * | 2018-11-30 | 2019-04-26 | 北京林业大学 | A kind of solidification processing method and products therefrom of lignin-base fiber |
| CN109680363B (en) * | 2018-11-30 | 2021-06-01 | 北京林业大学 | Curing treatment method of lignin-based fiber and obtained product |
| CN112973631A (en) * | 2021-02-20 | 2021-06-18 | 上海毅蓝电子科技有限公司 | Preparation method of activated carbon filter element for filtering total organic carbon in electroplating solution |
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