CN105274656A - Wood mesoporous activated carbon precursor and preparation method thereof - Google Patents
Wood mesoporous activated carbon precursor and preparation method thereof Download PDFInfo
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Abstract
The invention provides wood mesoporous activated carbon fiber and a preparation method of precursors of wood mesoporous activated carbon fiber, particularly relates to preparation of mesoporous activated carbon fiber and precursors of the wood mesoporous activated carbon fiber from liquefaction products of biomass resources such as wood and further relates to a novel pore forming agent for preparation of the mesoporous activated carbon fiber and a pore regulation technique used in the activation process. According to the novel mesoporous activated carbon fiber prepared from the liquefaction products of biomass materials with the technique, the mesoporosity can reach 55%-86% and is higher than that of existing products. Besides, home-made biomass activated carbon is taken as the mesopore forming agent, so that the mesopore forming agent is low in price, good in quality and free of secondary pollution and has a remarkable mesopore forming effect. Moreover, biomass resources are taken as double raw materials for preparation of mesoporous activated carbon fiber, the production cost is reduced, and the mesoporous activated carbon fiber is very competitive in the market.
Description
Technical field
The invention provides the preparation method of a kind of wooden mesopore activated carbon precursor and fiber, specifically, that one utilizes the biomass resource liquefied substances such as timber to prepare center hole activated carbon fiber, the invention still further relates to for the preparation of center hole activated carbon fiber Novel perforation agent used, and the hole control technique in activation process.
Background technology
Activated carbon fiber is also known as fibrous activated carbon, and being the new and effective sorbing material of one and environment-friendly engineering material that grow up nineteen sixties, is the third generation active adsorbing material after powdery and granular active carbon.Compared with granular or powdered activated carbon, activated carbon fiber has many good qualities, and its diameter is thin, pore structure is enriched, adsorption capacity is large, the de-speed of suction is fast, regenerate easily, high to the adsorption efficiency of low concentration.Little, easy process is damaged in the filter of active carbon fibre fiber products in addition, impurity is few, degree of purification is high, have good adsorbance and adsorption rate faster, and purification efficiency is high to the organic matter in organic and inorganic gas and liquid phase and precious metal ion.The most important thing is the mechanical and physical performance with general fibre, the fibre of different shape can be processed into freely, also can with other functional fibre compound uses so that design various absorption and the filter of small compact more, for practical application brings larger facility.So, apply activated carbon fiber and goods thereof in fields such as environmental protection, food, chemical industry chemistry, health care, Aero-Space, defence and military, atomic energy, daily life and weavings at present.
Most of activated carbon fiber is mainly based on micropore.Microcellular structure imparts the high specific area of activated carbon fiber, and high-specific surface area ensure that outstanding absorption property, and make activated carbon fiber in gaseous contamination, be subject to very large favor, but in the application of reality, it not generally the material of single needs absorption when adsorbing, at this moment the application of the activated carbon fiber of single micropore will greatly be limited, particularly to the absorption of some macromolecular substances, restriction suffered by micro porous activated carbon fiber is more and more obvious, therefore great for the application value of activated carbon fiber to preparing the activated carbon fiber with a large amount of mesopore hole.
At present, the raw materials of activated carbon fiber mainly based on fossil resource as viscose glue base, polyacrylonitrile-radical, asphaltic base, phenolic aldehyde base etc., but along with the exhaustion day by day of fossil resource, what ball ecological environment polluted increasingly sharpens, and the new exploitation with the raw material resources of sustainable use becomes important all the more.In addition, for improving the mesoporous of activated carbon fiber, researcher employs a large amount of perforating agents, as KOH, FeSO
4, TiO
2, MgO, AgNO
3, Co
+deng.Because the organic metal adopted is as mesopore promoter, metal ion that can not be necessary is inevitably introduced in final products, make it when application and development is in particular as catalyst carrier and medical material, likely can cause adverse consequences, and too increase the production cost of center hole activated carbon fiber.
The present inventor with biomass resources such as timber for raw material, its liquefaction products is utilized to be prepared into spinning solution, in the process of spinning, add biological active granulated charcoal as perforating agent, then prepare the wood activated charcoal fiber containing a large amount of mesopore through series of process such as spinning, solidification, activation.The method not only overcomes the residue problem of metal perforating agent, and the main source using biomass resource as active carbon fibre peacekeeping perforating agent raw material, reduce the production cost of center hole activated carbon fiber, improve biomass resource utilization rate and value-added content of product, and the wooden center hole activated carbon fiber mesoporous of preparation reaches more than 80%, substantially increases the generation of mesopore.
Summary of the invention
The object of this invention is to provide one utilizes the biomass liquefying things such as timber to prepare wooden center hole activated carbon fiber, and the main raw material of this center hole activated carbon fiber is based on biomass resources such as timber.
First the biological materials such as timber are synthesized spinning solution through post liquefaction by the present invention, then add perforating agent be spun into precursor through solidification, activation obtain center hole activated carbon fiber.
Therefore, another object of the present invention is to provide a kind of perforating agent that can be used for manufacturing a large amount of mesopore.
Technical scheme of the present invention is as follows:
A preparation method for wooden mesopore activated carbon precursor, step is as follows:
1) biomass material is ground into powder, adds phenol, carry out liquefaction reaction with phosphoric acid as catalyst, obtain liquefied substance;
2) add synthetics by liquefied substance weight 3 ~ 6%, from room temperature through 20 ~ 50min constant-speed heating to synthesis temperature 100 ~ 130 DEG C, reaction 2 ~ 10min, obtains spinning solution;
3) will add perforating agent active carbon in spinning solution, perforating agent adds by 0.5 ~ 2.5% of spinning solution weight, after mixing, puts into spinning machine 120 ~ 150 DEG C of melt spinnings and obtains precursor.
Described phenol is incorporated as raw material weight 4 ~ 6 times.
Described phosphoric acid addition is the concentration of 6% ~ 8% of phenol weight is 85% phosphoric acid.
Described liquefaction reaction, for stir in 150 DEG C ~ 160 DEG C at ambient pressure, reacts 2.5 ~ 3h.
Described synthetics is one or more in paraformaldehyde, furfural, hexamethylenetetramine or metaformaldehyde.
Described biomass material is timber, bamboo wood, stalk or string etc.; By biomass material in pulverizing, the fineness of material powder is with 20 ~ 80 orders.
Described perforating agent method for preparation of active carbon:
1) biomass material is ground into powder, granular size is with 200 ~ 300nm;
2) biomass material powder is put into activation furnace, at N
2be uniformly heated to 400 ~ 600 DEG C with the programming rate of 2 ~ 5 DEG C/min under protection, then naturally cool to room temperature with after 6 ~ 10g/min steam activation, 30 ~ 60min, obtain perforating agent activated carbon from activated sludge.
Spin the precursor obtained and do solidification process, concrete curing is: immersed by precursor in the acid solution of aldehyde, is heated to 85 ~ 97 DEG C with the programming rate of 10 ~ 25 DEG C/h, then at 80 ~ 97 DEG C of solidification 1 ~ 4h.
Utilize precursor to prepare the method for wooden center hole activated carbon fiber, the precursor after solidification is put into retort, at N
2carry out under protection carbonizing, obtain wooden center hole activated carbon fiber after activation processing.
The hole regulate and control method of wooden center hole activated carbon fiber, is precursor at N
2be uniformly heated to 700 ~ 900 DEG C with the programming rate of 2 ~ 5 DEG C/min under protection, after charing 30min, logical 6 ~ 10g/min steam carries out the wooden center hole activated carbon fiber that activation processing 30 ~ 60min can obtain different mesoporous.
Center hole activated carbon fiber prepared by the inventive method, has following characteristics:
Specific area: 967 ~ 2604 (m
2/ g),
Mesoporous: 55 ~ 86 (%),
Yield: 17 ~ 45 (%),
Average pore size: 1.95 ~ 2.08 (nm).
The present inventor is according to the characteristic of biological material, application liquefaction technology and carbonization-activation technology, through large quantity research and test, adopt the Novel center hole activated carbon fiber that the technology of the present invention utilizes biological material liquefied substance to prepare, its mesoporous can reach 55 ~ 86%, and the mesoporous of its Performance Ratio this product existing is all high.In addition, this invention utilizes homemade activated carbon from activated sludge as mesopore perforating agent, has of high quality and at a reasonable price, drilling successful, non-secondary pollution.Meanwhile, this technology, using biomass resource as the dual raw material of center hole activated carbon fiber, reduces production cost, commercially has very strong competitiveness.
Accompanying drawing explanation
Fig. 1: wooden center hole activated carbon fiber precursor;
Fig. 2: wooden center hole activated carbon fiber.
Detailed description of the invention
Spinning solution of the present invention, prepared by following method:
1) biomass materials such as timber are ground into powder, add phenol, carry out liquefaction process with phosphoric acid as catalyst, obtain liquefied substance;
2) add synthetics by liquefied substance weight 3 ~ 6%, from room temperature through 20 ~ 50min constant-speed heating to synthesis temperature 100 ~ 130 DEG C, reaction 2 ~ 10min, obtains spinning solution;
Researcher of the present invention finds through development test for many years, the catalytic performance of phosphoric acid in inorganic acid catalyst is best, so adopt phosphoric acid to carry out liquefaction process to biomass materials such as timber, be specially: Wooden Biomass raw meal is broken into powder, add the phenol of raw material weight 4 ~ 6 times and to be equivalent to the concentration that phenol adds 6% ~ 8% of weight be the phosphoric acid catalyst of 85%, stir at ambient pressure in 150 DEG C ~ 160 DEG C reaction 2.5 ~ 3h, obtain liquefied substance.Liquefaction process can be carried out under conventional liquefying plant.
Wherein, described synthetics can be one or more in paraformaldehyde, furfural, hexamethylenetetramine, metaformaldehyde.
Wherein, the biomass materials such as described available timber can be timber, bamboo wood, stalk, string etc.The fineness of described material powder is advisable with 20 ~ 80 orders (mesh screen aperture 0.9 ~ 0.18mm), biomass material can be pulverized in pulverizer and form.
Above-mentioned liquefaction process can be carried out under conventional liquefying plant.
To add homemade perforating agent active carbon in the spinning solution of above-mentioned acquisition, perforating agent adds by 0.5 ~ 2.5% of spinning solution weight, after mixing, puts into spinning machine 120 ~ 150 DEG C of melt spinnings and obtains precursor.
The present invention's perforating agent of the present invention, prepared by following method:
1) biomass materials such as timber are ground into powder, granular size is advisable with 200 ~ 300nm;
2) the biomass material powder such as timber puts into activation furnace, at N
2(N under protection
2flow is 60 ~ 100mL/min) be uniformly heated to 400 ~ 600 DEG C with the programming rate of 2 ~ 5 DEG C/min, then naturally cool to room temperature with after 6 ~ 10g/min steam activation, 30 ~ 60min, obtain perforating agent activated carbon from activated sludge;
Spin the precursor obtained and do solidification process, concrete curing is: immersed by precursor in the acid solution of aldehyde, is heated to 85 ~ 97 DEG C with the programming rate of 10 ~ 25 DEG C/h, then at 80 ~ 97 DEG C of solidification 1 ~ 4h.
The acid solution of above-mentioned aldehyde can be the oxalic acid solution of the formaldehyde of 18.5%, also can be the hydrochloric acid solution of the formaldehyde of 18.5%.
Further, the above-mentioned precursor prepared is obtained wooden center hole activated carbon fiber through carbonization/activation by the present invention, and its concrete grammar is: precursor is put into retort, at N
2(N under protection
2flow is 60 ~ 100mL/min) be uniformly heated to 700 ~ 900 DEG C with the programming rate of 2 ~ 5 DEG C/min, after charing 30min, logical 6 ~ 10g/min steam carries out activation processing 30 ~ 60min then cool to room temperature, obtains wooden center hole activated carbon fiber.
Embodiment is for illustration of the present invention below, but is not used for limiting the scope of the invention.
Embodiment 1
Fir powder is broken into the powder of 80 orders (mesh screen aperture 0.18mm), be then 8% of phenol addition by the phenol of 4 times of this wood powder and wood weight and catalyst phosphoric acid (phosphoric acid concentration is 85%) addition) join in three mouthfuls of vials, be placed in the oil bath being preheated to 160 DEG C in advance, install condenser, start agitating device (rotating speed 1058rpm) to liquefy, liquefying time is 2.5 hours, obtains liquefied substance.
Meanwhile, 200nm timber powder is put into activation furnace, at 60mL/minN
2being uniformly heated to 400 DEG C with the programming rate of 2 DEG C/min under protection, then obtaining perforating agent activated carbon from activated sludge with naturally cooling after 6g/min steam activation 30min.
Get the paraformaldehyde that timber liquefied matter adds liquefied substance weight 3%, from room temperature through 20min constant-speed heating to 100 DEG C, reaction 2min, obtain the liquefied spinning liquid of spinning.In spinning solution, add the perforating agent active carbon of homemade 1%, after mixing, put into spinning machine 120 DEG C of melt spinnings and obtain precursor (see Fig. 1).
Precursor is immersed by concentration be respectively 12% formaldehyde and 18.5% the aqueous solution of mass percent that form of hydrochloric acid in, be heated to 85 DEG C with the programming rate of 10 DEG C/h, then process 1h 80 DEG C of solidifications.
Precursor after solidification is put into retort, at N
2(N under protection
2flow is 100mL/min) be uniformly heated to 800 DEG C with the programming rate of 2 DEG C/min, after charing 30min, logical 10g/min steam carries out activation processing 30min then cool to room temperature, obtains wooden center hole activated carbon fiber (see Fig. 2).
The specific area prepared: 2048m
2/ g; Mesoporous: 78%; Yield: 33%.
Embodiment 2
Mao bamboon is ground into 60 object powder, be then 6% of phenol addition by the phenol of 6 times of this mao bamboon powder and mao bamboon weight and catalyst phosphoric acid (phosphoric acid concentration is 85%) addition) join in three mouthfuls of vials, be placed in the oil bath being preheated to 150 DEG C in advance, install condenser, start agitating device (rotating speed 1058rpm) to liquefy, liquefying time is 3 hours, obtains liquefied substance.
Meanwhile, 300nm timber powder is put into activation furnace, at 100mL/minN
2being uniformly heated to 600 DEG C with the programming rate of 5 DEG C/min under protection, then obtaining perforating agent activated carbon from activated sludge with naturally cooling after 10g/min steam activation 60min.
Get liquefied substance and add furfural by liquefied substance weight 5%, from room temperature through 40min constant-speed heating to 120 DEG C, reaction 5min, obtains the liquefied spinning liquid of spinning.In spinning solution, add the perforating agent active carbon of homemade 2%, after mixing, put into spinning machine 140 DEG C of melt spinnings and obtain precursor (see Fig. 1).
Precursor is immersed by concentration be respectively 12% formaldehyde and 18.5% the aqueous solution of mass percent that form of hydrochloric acid in, be heated to 95 DEG C with the programming rate of 20 DEG C/h, then process 2h 95 DEG C of solidifications.
Precursor after solidification is put into retort, at N
2(N under protection
2flow is 100mL/min) be uniformly heated to 850 DEG C with the programming rate of 5 DEG C/min, after charing 30min, logical 8g/min steam carries out activation processing 60min then cool to room temperature, obtains wooden center hole activated carbon fiber (see Fig. 2).
The specific area prepared: 2604m
2/ g; Mesoporous: 86%; Yield: 17%.
Embodiment 3
Cotton stalk is ground into 40 object powder, be then 8% of phenol addition by the phenol of 4 times of this cotton stalk powder and cotton stalk weight and catalyst phosphoric acid (phosphoric acid concentration is 85%) addition) join in three mouthfuls of vials, be placed in the oil bath being preheated to 160 DEG C in advance, install condenser, start agitating device (rotating speed 1058rpm) to liquefy, liquefying time is 2.5 hours, obtains liquefied substance.
Meanwhile, 250nm timber powder is put into activation furnace, at 80mL/minN
2being uniformly heated to 500 DEG C with the programming rate of 3 DEG C/min under protection, then obtaining perforating agent activated carbon from activated sludge with naturally cooling after 8g/min steam activation 45min.
Get liquefied substance with by the hexamethylenetetramine of liquefaction products weight 6% and metaformaldehyde mixture (arbitrarily than), be uniformly heated to synthesis temperature 130 DEG C from room temperature through 50min, reaction 10min, obtains the liquefied spinning liquid of spinning.In spinning solution, add the perforating agent active carbon of homemade 1.5%, after mixing, put into spinning machine 150 DEG C of melt spinnings and obtain precursor (see Fig. 1).
Carbon fiber precursors prepared from liquefied is immersed by concentration be respectively 18.5% formaldehyde and 18.5% the aqueous solution of mass percent that form of hydrochloric acid in, be heated to 97 DEG C with the programming rate of 25 DEG C/h, then process 4h 97 DEG C of solidifications.
Precursor after solidification is put into retort, at N
2(N under protection
2flow is 80mL/min) be uniformly heated to 750 DEG C with the programming rate of 4 DEG C/min, after charing 30min, logical 6g/min steam carries out activation processing 45min then cool to room temperature, obtains wooden center hole activated carbon fiber (see Fig. 2).
The specific area prepared: 1172m
2/ g; Mesoporous: 64%; Yield: 38%.
Embodiment 4
Chinese white poplar is ground into 20 object powder, be then 6% of phenol addition by the phenol of 3 times of this wood powder and wood weight and catalyst phosphoric acid (phosphoric acid concentration is 85%) addition) join in three mouthfuls of vials, be placed in the oil bath being preheated to 150 DEG C in advance, install condenser, start agitating device (rotating speed 1058rpm) to liquefy, liquefying time is 2.5 hours, obtains liquefied substance.
Meanwhile, 250nm timber powder is put into activation furnace, at 60mL/minN
2being uniformly heated to 550 DEG C with the programming rate of 4 DEG C/min under protection, then obtaining perforating agent activated carbon from activated sludge with naturally cooling after 8g/min steam activation 45min.
Get liquefied substance and the hexamethylenetetramine by liquefaction products weight 6%, be uniformly heated to synthesis temperature 130 DEG C from room temperature through 40min, reaction 10min, obtains the liquefied spinning liquid of spinning.In spinning solution, add the perforating agent active carbon of homemade 1.0%, after mixing, put into spinning machine 130 DEG C of melt spinnings and obtain precursor (see Fig. 1).
Carbon fiber precursors prepared from liquefied is immersed by concentration be respectively 18.5% formaldehyde and 18.5% the aqueous solution of mass percent that form of hydrochloric acid in, be heated to 97 DEG C with the programming rate of 25 DEG C/h, then process 3h 97 DEG C of solidifications.
Precursor after solidification is put into retort, at N
2(N under protection
2flow is 60mL/min) be uniformly heated to 700 DEG C with the programming rate of 3 DEG C/min, after charing 30min, logical 8g/min steam carries out activation processing 45min then cool to room temperature, obtains wooden center hole activated carbon fiber (see Fig. 2).
The specific area prepared: 967m
2/ g; Mesoporous: 55%; Yield: 45%.
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, not departing from the these modifications or improvements substantially of spirit of the present invention, all the scope of protection of present invention is belonged to.
Claims (8)
1. a preparation method for wooden mesopore activated carbon precursor, is characterized in that step is as follows:
1) biomass material is ground into powder, adds phenol, carry out liquefaction reaction with phosphoric acid as catalyst, obtain liquefied substance;
2) add synthetics by liquefied substance weight 3 ~ 6%, from room temperature through 20 ~ 50min constant-speed heating to synthesis temperature 100 ~ 130 DEG C, reaction 2 ~ 10min, obtains spinning solution;
3) will add perforating agent active carbon in spinning solution, perforating agent adds by 0.5 ~ 2.5% of spinning solution weight, after mixing, puts into spinning machine 120 ~ 150 DEG C of melt spinnings and obtains precursor.
2. the method for claim 1, is characterized in that described phenol is incorporated as raw material weight 4 ~ 6 times.
3. the method for claim 1, is characterized in that described phosphoric acid addition be the concentration of 6% ~ 8% of phenol weight is 85% phosphoric acid.
4. the method for claim 1, is characterized in that described liquefaction reaction is for stir in 150 DEG C ~ 160 DEG C at ambient pressure, reaction 2.5 ~ 3h.
5. the method for claim 1, is characterized in that described synthetics is one or more in paraformaldehyde, furfural, hexamethylenetetramine or metaformaldehyde.
6. the method for claim 1, is characterized in that described biomass material is timber, bamboo wood, stalk or string; By biomass material in pulverizing, the fineness of material powder is with 20 ~ 80 orders.
7. the method for claim 1, is characterized in that described perforating agent method for preparation of active carbon:
1) biomass material is ground into powder, granular size is with 200 ~ 300nm;
2) biomass material powder is put into activation furnace, at N
2be uniformly heated to 400 ~ 600 DEG C with the programming rate of 2 ~ 5 DEG C/min under protection, then naturally cool to room temperature with after 6 ~ 10g/min steam activation, 30 ~ 60min, obtain perforating agent activated carbon from activated sludge.
8. utilize the precursor of claim 1 to prepare the method for wooden center hole activated carbon fiber, it is characterized in that precursor being put into retort, at N
2be uniformly heated to 700 ~ 900 DEG C with the programming rate of 2 ~ 5 DEG C/min under protection, after charing 30min, logical 6 ~ 10g/min steam carries out activation processing 30 ~ 60min then cool to room temperature, obtains wooden center hole activated carbon fiber.
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Cited By (3)
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| CN107313131A (en) * | 2017-07-18 | 2017-11-03 | 成都新柯力化工科技有限公司 | The active carbon filament environment-friendly materials and preparation method of a kind of rapid classification purification air |
| 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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