CN105274656B - A kind of preparation method of wooden mesopore activated carbon precursor and fiber - Google Patents
A kind of preparation method of wooden mesopore activated carbon precursor and fiber Download PDFInfo
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- CN105274656B CN105274656B CN201510683105.6A CN201510683105A CN105274656B CN 105274656 B CN105274656 B CN 105274656B CN 201510683105 A CN201510683105 A CN 201510683105A CN 105274656 B CN105274656 B CN 105274656B
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Abstract
The invention provides a kind of wooden center hole activated carbon fiber and its preparation method of precursor, specifically, it is that one kind prepares center hole activated carbon fiber and its precursor using biomass resource liquefied substances such as timber, the invention further relates to the Novel perforation agent for being used to prepare used by center hole activated carbon fiber, and the hole control technique in activation process.The novel center hole activated carbon fiber prepared using biological material liquefied substance using the technology of the present invention, its mesoporous can reach 55~86%, and its performance is all higher than the mesoporous of the existing product.In addition, the invention is by the use of homemade activated carbon from activated sludge as mesopore perforating agent, with of high quality and at a reasonable price, drilling effect substantially, non-secondary pollution.Meanwhile, the technology reduces production cost using biomass resource as the dual raw material of center hole activated carbon fiber, commercially with very strong competitiveness.
Description
Technical field
It is a kind of profit specifically the invention provides a kind of wooden mesopore activated carbon precursor and the preparation method of fiber
Center hole activated carbon fiber is prepared with the biomass resource liquefied substance such as timber, the invention further relates to be used to prepare center hole activated carbon fiber
Novel perforation agent used, and the hole control technique in activation process.
Background technology
NACF is also known as fibrous activated carbon, is a kind of new and effective suction for growing up nineteen sixties
Enclosure material and environment-friendly engineering material, are the third generation active adsorbing materials after powdery and granular active carbon.With granular or powder
Shaped activated carbon is compared, and NACF has many good qualities, its diameter is thin, pore structure abundant, adsorption capacity is big, it is fast to inhale de- speed,
Regeneration is easy, and the adsorption efficiency to low concentration is high.Other active carbon fibre fiber products filter damage is small, be easily processed, impurity is few, purification journey
Degree is high, has preferable adsorbance to the organic matter and precious metal ion in organic and inorganic gas and liquid phase and adsorbs faster
Speed, and purification efficiency is high.Above all the mechanical and physical performance with general fibre, can freely be processed into difference
The fibre of form, can also use with other functions fiber composite, in order to design the various absorption of more small compact
And filter, it is that practical application brings bigger facility.So, defended in environmental protection, food, chemical industry chemistry, medical treatment at present
The fields such as life, Aero-Space, defence and military, atomic energy, daily life and weaving apply NACF and its product.
Most of NACFs are main based on micropore.Microcellular structure imparts NACF specific surface area high,
And high-specific surface area ensure that outstanding absorption property, and cause that NACF is subject to very big green grass or young crops in terms of gaseous contamination
Look at, but in actual application, be generally not when being adsorbed it is single the need for the material that adsorbs, the at this moment activity of single micropore
The application of Carbon fibe will be limited greatly, particularly to the absorption of some macromolecular substances, micro porous active carbon fibre
The suffered limitation of dimension is more and more obvious, therefore to preparing the NACF with a large amount of mesopore holes for NACF
Application value it is great.
At present, the preparing raw material of NACF is main with fossil resource such as viscose glue base, polyacrylonitrile-radical, asphaltic base, phenol
Based on aldehyde radical etc., but with the increasingly depleted of fossil resource, ball ecological environment pollution increasingly sharpens, new with sustainable
The exploitation of the raw material resources for utilizing becomes important all the more.In addition, being the mesoporous of raising NACF, researcher has used greatly
The perforating agent of amount, such as KOH, FeSO4、TiO2、MgO、AgNO3、Co+Deng.Because the organic metal for using is used as mesopore accelerator,
In final products inevitably introduce can not necessary metal ion, be allowed to be particularly as catalyst carrier in application and development
During with medical material, it is possible to adverse consequences can be caused, and also increase the production cost of center hole activated carbon fiber.
The present inventor is prepared into spinning solution, in spinning with biomass resources such as timber as raw material using its liquefaction products
During add biological active granulated charcoal as perforating agent, then by the series of process such as spinning, solidification, activation prepare containing
The wood activated charcoal fiber of a large amount of mesopores.The method not only overcomes the residue problem of metal perforating agent, and with biomass resource
As the main source of active carbon fibre peacekeeping perforating agent raw material, the production cost of center hole activated carbon fiber is reduced, improve biological
Matter resource utilization and value-added content of product, and the wooden center hole activated carbon fiber mesoporous for preparing are up to more than 80%, significantly
Improve the generation of mesopore.
The content of the invention
Wooden center hole activated carbon fiber is prepared using biomass liquefying things such as timber it is an object of the invention to provide one kind, should
The primary raw material of center hole activated carbon fiber is based on the biomass resources such as timber.
The biological materials such as timber are synthesized spinning solution by the present invention after liquefaction first, are added perforating agent and are spun into precursor
Cured, activation obtains center hole activated carbon fiber.
Therefore, it is a further object to provide a kind of perforating agent that can be used to manufacture a large amount of mesopores.
Technical scheme is as follows：
A kind of preparation method of wooden mesopore activated carbon precursor, step is as follows：
1) biomass material is ground into powder, adds phenol, liquefaction reaction is carried out as catalyst with phosphoric acid, must liquefied
Thing；
2) by the addition synthetics of liquefied substance weight 3~6%, from room temperature through 20~50min constant-speed heatings to synthesis temperature
100~130 DEG C, 2~10min is reacted, obtain spinning solution；
3) perforating agent activated carbon, perforating agent will be added 0.5~2.5% addition of spinning solution weight, mixing is pressed in spinning solution
After uniform, 120~150 DEG C of melt spinnings obtain precursor in being put into spinning-drawing machine.
Described phenol is incorporated as 4~6 times of raw material weight.
Described phosphoric acid addition is 85% phosphoric acid for the 6%~8% of phenol weight concentration.
Described liquefaction reaction reacts 2.5~3h to stir at ambient pressure in 150 DEG C~160 DEG C.
Described synthetics is one or more in paraformaldehyde, furfural, hexamethylenetetramine or metaformaldehyde.
Described biomass material is timber, bamboo wood, stalk or string etc.；Biomass material is being crushed, raw material
The fineness of powder is with 20~80 mesh.
Described perforating agent method for preparation of active carbon：
1) biomass material is ground into powder, granule size with 200~300nm；
2) biomass material powder is put into activation furnace, in N2Uniformly added with the programming rate of 2~5 DEG C/min under protection
Heat, then with room temperature is naturally cooled to after 6~10g/min steam activations, 30~60min, obtains perforating agent to 400~600 DEG C
Activated carbon from activated sludge.
The precursor that spinning is obtained makees curing process, and specific curing is：Precursor is immersed in the acid solution of aldehyde, with 10
The programming rate of~25 DEG C/h is heated to 85~97 DEG C, then solidifies 1~4h at 80~97 DEG C.
The method that wooden center hole activated carbon fiber is prepared using precursor, the precursor after solidification is put into retort, in N2
Carbonized under protection, obtained wooden center hole activated carbon fiber after activation process.
The hole regulation and control method of wooden center hole activated carbon fiber, is in N by precursor2With the liter of 2~5 DEG C/min under protection
Warm speed is uniformly heated to 700~900 DEG C, and leading to 6~10g/min vapor after charing 30min carries out 30~60min of activation process
The wooden center hole activated carbon fiber of different mesoporous can be obtained.
Center hole activated carbon fiber prepared by the inventive method, has the characteristics that：
Specific surface area：967~2604 (m2/ g),
Mesoporous：55~86 (%),
Yield：17~45 (%),
Average pore size：1.95~2.08 (nm).
The present inventor according to the characteristic of biological material, using liquefaction technology and carbonization-activation technology, by numerous studies
And experiment, the novel center hole activated carbon fiber prepared using biological material liquefied substance using the technology of the present invention, its mesoporous can
55~86% are reached, its performance is all higher than the mesoporous of the existing product.In addition, the invention utilizes homemade activated carbon from activated sludge
As mesopore perforating agent, with of high quality and at a reasonable price, drilling effect substantially, non-secondary pollution.Meanwhile, the technology is made with biomass resource
It is the dual raw material of center hole activated carbon fiber, reduces production cost, commercially with very strong competitiveness.
Brief description of the drawings
Fig. 1：Wooden center hole activated carbon fiber precursor；
Fig. 2：Wooden center hole activated carbon fiber.
Specific embodiment
Spinning solution of the present invention, is prepared by following methods：
1) biomass materials such as timber are ground into powder, add phenol, liquefaction treatment is carried out as catalyst with phosphoric acid,
Obtain liquefied substance；
2) by the addition synthetics of liquefied substance weight 3~6%, from room temperature through 20~50min constant-speed heatings to synthesis temperature
100~130 DEG C, 2~10min is reacted, obtain spinning solution；
Researcher of the present invention has found that catalytic performance of the phosphoric acid in inorganic acid catalyst is most by development test for many years
It is good, so liquefaction treatment is carried out to biomass materials such as timber using phosphoric acid, specially：Wooden Biomass raw material is ground into
Powder, adds the phenol of 4~6 times of raw material weight and to add 6%~8% concentration of weight equivalent to phenol is that 85% phosphoric acid is urged
Agent, stirs react 2.5~3h in 150 DEG C~160 DEG C at ambient pressure, obtains liquefied substance.Liquefaction treatment can be in conventional liquefying plant
Under carry out.
Wherein, described synthetics can be one kind in paraformaldehyde, furfural, hexamethylenetetramine, metaformaldehyde or
It is various.
Wherein, the biomass material such as described available timber can be timber, bamboo wood, stalk, string etc..Institute
The fineness of material powder is stated to be advisable with 20~80 mesh (0.9~0.18mm of mesh screen aperture), can be by biomass material in pulverizer
Crushing is formed.
Above-mentioned liquefaction treatment can be carried out under conventional liquefying plant.
To add homemade perforating agent activated carbon in the spinning solution of above-mentioned acquisition, perforating agent press spinning solution weight 0.5~
2.5% adds, and after being well mixed, 120~150 DEG C of melt spinnings obtain precursor in being put into spinning-drawing machine.
Institute of the invention perforating agent of the present invention, is prepared by following methods：
1) biomass materials such as timber are ground into powder, granule size to be advisable with 200~300nm；
2) the biomass material powder such as timber is put into activation furnace, in N2(N under protection2Flow is 60~100mL/min) with
The programming rate of 2~5 DEG C/min is uniformly heated to 400~600 DEG C, then with 6~10g/min steam activations, 30~60min
After naturally cool to room temperature, obtain perforating agent activated carbon from activated sludge；
The precursor that spinning is obtained makees curing process, and specific curing is：Precursor is immersed in the acid solution of aldehyde, with 10
The programming rate of~25 DEG C/h is heated to 85~97 DEG C, then solidifies 1~4h at 80~97 DEG C.
The acid solution of above-mentioned aldehyde can be the oxalic acid solution of 18.5% formaldehyde, or the hydrochloric acid of 18.5% formaldehyde
Solution.
Further, the above-mentioned precursor for preparing is obtained wooden center hole activated carbon fiber by the present invention through carbonization/activation, its
Specific method is：Precursor is put into retort, in N2(N under protection2Flow is 60~100mL/min) with 2~5 DEG C/min's
Programming rate is uniformly heated to 700~900 DEG C, lead to after charing 30min 6~10g/min vapor carry out activation process 30~
Then 60min is cooled to room temperature, obtains wooden center hole activated carbon fiber.
Example below is used to illustrate the present invention, but is not limited to the scope of the present invention.
Embodiment 1
China fir is ground into the powder of 80 mesh (mesh screen aperture 0.18mm), then by 4 times of the wood powder and wood weight
Phenol and catalyst phosphoric acid (phosphoric acid concentration is 85%) addition are the 8% of phenol addition) it is added in three mouthfuls of vials, put
In 160 DEG C of oil bath is preheated in advance, condenser is installed, start agitating device (rotating speed 1058rpm) and liquefied, liquefied
Time is 2.5 hours, obtains liquefied substance.
Meanwhile, 200nm wood powders are put into activation furnace, in 60mL/min N2With the intensification speed of 2 DEG C/min under protection
Degree is uniformly heated to 400 DEG C, then obtains perforating agent biomass active with natural cooling after 6g/min steam activations 30min
Charcoal.
The paraformaldehyde that timber liquefied matter adds liquefied substance weight 3% is taken, from room temperature through 20min constant-speed heatings to 100 DEG C,
Reaction 2min, obtains the liquefied spinning liquid of spinning.Homemade 1% perforating agent activated carbon is added in spinning solution, is mixed
After uniform, 120 DEG C of melt spinnings obtain precursor in being put into spinning-drawing machine (see Fig. 1).
Precursor immersion is respectively the aqueous solution of the mass percent that 12% formaldehyde and 18.5% hydrochloric acid are constituted by concentration
In, 85 DEG C are heated to the programming rate of 10 DEG C/h, then in 80 DEG C of curing process 1h.
Precursor after solidification is put into retort, in N2(N under protection2Flow is 100mL/min) with the liter of 2 DEG C/min
Warm speed is uniformly heated to 800 DEG C, after charing 30min, and logical 10g/min vapor carries out activation process 30min and then is cooled to
Room temperature, obtains wooden center hole activated carbon fiber (see Fig. 2).
The specific surface area for preparing：2048m2/g；Mesoporous：78%；Yield：33%.
Embodiment 2
Mao bamboon is ground into the powder of 60 mesh, then the phenol and catalyst phosphorus by the mao bamboon powder with 6 times of mao bamboon weight
Sour (phosphoric acid concentration is 85%) addition is the 6% of phenol addition) it is added in three mouthfuls of vials, it is placed in and is preheated in advance
In 150 DEG C of oil bath, condenser is installed, starts agitating device (rotating speed 1058rpm) and liquefied, liquefying time is 3 hours,
Obtain liquefied substance.
Meanwhile, 300nm wood powders are put into activation furnace, in 100mL/min N2With the intensification of 5 DEG C/min under protection
Speed is uniformly heated to 600 DEG C, and then obtaining perforating agent biomass with natural cooling after 10g/min steam activations 60min lives
Property charcoal.
Take liquefied substance and add furfural with by liquefied substance weight 5%, from room temperature through 40min constant-speed heatings to 120 DEG C, reaction
5min, obtains the liquefied spinning liquid of spinning.Homemade 2% perforating agent activated carbon is added in spinning solution, is well mixed
Afterwards, 140 DEG C of melt spinnings obtain precursor in being put into spinning-drawing machine (see Fig. 1).
Precursor immersion is respectively the aqueous solution of the mass percent that 12% formaldehyde and 18.5% hydrochloric acid are constituted by concentration
In, 95 DEG C are heated to the programming rate of 20 DEG C/h, then in 95 DEG C of curing process 2h.
Precursor after solidification is put into retort, in N2(N under protection2Flow is 100mL/min) with the liter of 5 DEG C/min
Warm speed is uniformly heated to 850 DEG C, after charing 30min, and logical 8g/min vapor carries out activation process 60min and then is cooled to room
Temperature, obtains wooden center hole activated carbon fiber (see Fig. 2).
The specific surface area for preparing：2604m2/g；Mesoporous：86%；Yield：17%.
Embodiment 3
Cotton stalk powder is broken into the powder of 40 mesh, then the phenol and catalyst phosphorus by the cotton stalk powder with 4 times of cotton stalk weight
Sour (phosphoric acid concentration is 85%) addition is the 8% of phenol addition) it is added in three mouthfuls of vials, it is placed in and is preheated in advance
In 160 DEG C of oil bath, condenser is installed, start agitating device (rotating speed 1058rpm) and liquefied, liquefying time is 2.5 small
When, obtain liquefied substance.
Meanwhile, 250nm wood powders are put into activation furnace, in 80mL/min N2With the intensification speed of 3 DEG C/min under protection
Degree is uniformly heated to 500 DEG C, then obtains perforating agent biomass active with natural cooling after 8g/min steam activations 45min
Charcoal.
Liquefied substance and the hexamethylenetetramine and metaformaldehyde mixture (any ratio) by liquefaction products weight 6% are taken, from
Room temperature is uniformly heated to 130 DEG C of synthesis temperature through 50min, reacts 10min, obtains the liquefied spinning liquid of spinning.In spinning
Homemade 1.5% perforating agent activated carbon is added in liquid, after being well mixed, 150 DEG C of melt spinnings obtain original in being put into spinning-drawing machine
Silk (see Fig. 1).
Carbon fiber precursors prepared from liquefied immersion is respectively the quality that 18.5% formaldehyde and 18.5% hydrochloric acid are constituted by concentration
In the aqueous solution of percentage, 97 DEG C are heated to the programming rate of 25 DEG C/h, then in 97 DEG C of curing process 4h.
Precursor after solidification is put into retort, in N2(N under protection2Flow is 80mL/min) with the intensification of 4 DEG C/min
Speed is uniformly heated to 750 DEG C, after charing 30min, and logical 6g/min vapor carries out activation process 45min and then is cooled to room
Temperature, obtains wooden center hole activated carbon fiber (see Fig. 2).
The specific surface area for preparing：1172m2/g；Mesoporous：64%；Yield：38%.
Embodiment 4
Chinese white poplar is ground into the powder of 20 mesh, then the phenol and catalyst phosphorus by the wood powder with 3 times of wood weight
Sour (phosphoric acid concentration is 85%) addition is the 6% of phenol addition) it is added in three mouthfuls of vials, it is placed in and is preheated in advance
In 150 DEG C of oil bath, condenser is installed, start agitating device (rotating speed 1058rpm) and liquefied, liquefying time is 2.5 small
When, obtain liquefied substance.
Meanwhile, 250nm wood powders are put into activation furnace, in 60mL/min N2With the intensification speed of 4 DEG C/min under protection
Degree is uniformly heated to 550 DEG C, then obtains perforating agent biomass active with natural cooling after 8g/min steam activations 45min
Charcoal.
Liquefied substance and the hexamethylenetetramine by liquefaction products weight 6% are taken, synthesis is uniformly heated to through 40min from room temperature
130 DEG C of temperature, reacts 10min, obtains the liquefied spinning liquid of spinning.Homemade 1.0% drilling is added in spinning solution
Agent activated carbon, after being well mixed, 130 DEG C of melt spinnings obtain precursor in being put into spinning-drawing machine (see Fig. 1).
Carbon fiber precursors prepared from liquefied immersion is respectively the quality that 18.5% formaldehyde and 18.5% hydrochloric acid are constituted by concentration
In the aqueous solution of percentage, 97 DEG C are heated to the programming rate of 25 DEG C/h, then in 97 DEG C of curing process 3h.
Precursor after solidification is put into retort, in N2(N under protection2Flow is 60mL/min) with the intensification of 3 DEG C/min
Speed is uniformly heated to 700 DEG C, after charing 30min, and logical 8g/min vapor carries out activation process 45min and then is cooled to room
Temperature, obtains wooden center hole activated carbon fiber (see Fig. 2).
The specific surface area for preparing：967m2/g；Mesoporous：55%；Yield：45%.
Although above the present invention is described in detail with a general description of the specific embodiments,
On the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Cause
This, in the substantially these modifications or improvements without departing from spirit of the present invention, belongs to the scope of protection of present invention.
Claims (7)
1. a kind of preparation method of wooden mesopore activated carbon precursor, it is characterized in that step is as follows：
1) biomass material is ground into powder, adds phenol, liquefaction reaction is carried out as catalyst with phosphoric acid, obtain liquefied substance；
2) by the addition synthetics of liquefied substance weight 3~6%, from room temperature through 20~50min constant-speed heatings to synthesis temperature 100~
130 DEG C, 2~10min is reacted, obtain spinning solution；
3) perforating agent activated carbon, perforating agent will be added to press 0.5~2.5% addition of spinning solution weight, be well mixed in spinning solution
Afterwards, 120~150 DEG C of melt spinnings obtain precursor in being put into spinning-drawing machine；
Described perforating agent method for preparation of active carbon：
1) biomass material is ground into powder, granule size for 200~300nm；
2) biomass material powder is put into activation furnace, in N2It is uniformly heated to the programming rate of 2~5 DEG C/min under protection
400~600 DEG C, then with room temperature is naturally cooled to after 6~10g/min steam activations, 30~60min, obtain perforating agent biological
Activated carbon.
2. the method for claim 1, it is characterized in that described phenol addition is 4~6 times of raw material weight.
3. the method for claim 1, it is characterized in that described phosphoric acid addition for phenol weight 6%~8% it is dense
It is 85% phosphoric acid to spend.
4. the method for claim 1, it is characterized in that described liquefaction reaction to stir in 150 DEG C~160 at ambient pressure
DEG C, react 2.5~3h.
5. the method for claim 1, it is characterized in that described synthetics is paraformaldehyde, furfural, hexamethylenetetramine
Or one or more in metaformaldehyde.
6. the method for claim 1, it is characterized in that described biomass material is fine timber, bamboo wood, stalk or plant
Dimension.
7. the method for preparing wooden center hole activated carbon fiber using the precursor of claim 1, it is characterized in that precursor is put into charing
In stove, in N2700~900 DEG C are uniformly heated to the programming rate of 2~5 DEG C/min under protection, logical 6 after charing 30min~
10g/min vapor carries out 30~60min of activation process, is then cooled to room temperature, obtains wooden center hole activated carbon fiber.
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| CN111961222A (en) * | 2020-07-15 | 2020-11-20 | 天津科技大学 | Method for preparing gel elastomer based on wood liquefied product and gel elastomer |
| CN112592495A (en) * | 2021-01-05 | 2021-04-02 | 天津科技大学 | Preparation method of wood-based microspheres and activated carbon spheres thereof |
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|---|---|---|---|---|
| CN101135075A (en) * | 2007-10-11 | 2008-03-05 | 北京林业大学 | Wood liquefied carbide fiber, protofilament and preparation method thereof |
| CN102337143A (en) * | 2010-07-22 | 2012-02-01 | 重庆三峡农业科学院 | Carbonization method for straws |
| CN102719935A (en) * | 2012-06-07 | 2012-10-10 | 北京林业大学 | Preparation method of active wood-based carbon fibers |
| CN104724717A (en) * | 2015-02-13 | 2015-06-24 | 浙江皓翔矿业有限公司 | Preparation method of pyrophyllite-based microporous spherical powder and application thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101135075A (en) * | 2007-10-11 | 2008-03-05 | 北京林业大学 | Wood liquefied carbide fiber, protofilament and preparation method thereof |
| CN102337143A (en) * | 2010-07-22 | 2012-02-01 | 重庆三峡农业科学院 | Carbonization method for straws |
| CN102719935A (en) * | 2012-06-07 | 2012-10-10 | 北京林业大学 | Preparation method of active wood-based carbon fibers |
| CN104724717A (en) * | 2015-02-13 | 2015-06-24 | 浙江皓翔矿业有限公司 | Preparation method of pyrophyllite-based microporous spherical powder and application thereof |
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