CN102719935A - Preparation method of active wood-based carbon fibers - Google Patents
Preparation method of active wood-based carbon fibers Download PDFInfo
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- CN102719935A CN102719935A CN2012101872516A CN201210187251A CN102719935A CN 102719935 A CN102719935 A CN 102719935A CN 2012101872516 A CN2012101872516 A CN 2012101872516A CN 201210187251 A CN201210187251 A CN 201210187251A CN 102719935 A CN102719935 A CN 102719935A
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Abstract
The invention provides a preparation method of active wood-based carbon fibers. The method includes: placing wood powder into a liquefying plant, adding phenol and preparing a liquefied product in presence of acid catalysts; subjecting the wood liquefied product to spinning solution synthesis, melt spinning and curing process so that wood liquefied product protofilaments are prepared; and finally, placing the protofilaments into an activating device by means of a one-step physical activation method, namely, simultaneous proceeding of carbonization and activation, so that the final products, namely, the active wood carbon fibers are obtained. Compared with an existing method adopting biomass carbon fibers (such as viscose-based and lignin-based), the method using wood processing residua as raw materials has the advantages that chemical components such as celluloses and lignins do not need to be individually extracted from biomass but are completely used, so that production process is simplified, production cost is reduced, and use ratio of the biomass is increased.
Description
Technical field
The present invention relates to chemical field, specifically, relate to a kind of through " one-step method " the physically activated method for preparing active wooden carbon fiber.
Background technology
Activated carbon fiber is compared with granular active carbon with traditional powder as porous carbon materials, not only has high specific area, big, the fireballing characteristics of adsorption/desorption of adsorbance, can also process various goods and variform as required.Therefore, it is widely used in fields such as environment, chemical industry, food, health, electronics, electrochemistry.At present with regard to the activated carbon fiber raw material; Mainly be viscose, phenolic fibre, polyacrylonitrile, pitch fibers and aramid fiber; And mainly rely on fossil resource such as the raw material of polyacrylonitrile, pitch class etc.; Exhausted day by day based on fossil resource, reduce because of the exploitation fossil resource to the negative effect that ball ecological environment causes, carrying out biomass material, to prepare the research of activated carbon fiber imperative.
Summary of the invention
The purpose of this invention is to provide a kind of through " one-step method " the physically activated method for preparing active wooden carbon fiber.
In order to realize the object of the invention, the preparation method of the wooden carbon fiber of a kind of activity of the present invention, it is that wood powder is placed liquefying plant, adds phenol, under acid catalyst, prepares the thing that liquefies; Timber liquefied matter can make the timber liquefied matter precursor through synthetic, the melt spinning and the curing process of spinning solution; At last precursor is placed activating apparatus.The present invention adopts an one-step physical activation method, and promptly carbonization-activation carries out simultaneously, and through adjustment activation temperature, soak time, steam flow and heating rate, obtaining specific area is 740.50-2641.085m
2/ g, yield is the novel wooden activated carbon fiber of 10-48%.
The objective of the invention is to adopt following technical scheme to realize.Preparation method according to the wooden carbon fiber of a kind of activity provided by the invention may further comprise the steps: 1) wood powder is placed liquefying plant, to the phenol that wherein adds 4-6 times of wood powder weight; In the presence of acid catalyst; Be heated to 150-160 ℃, insulation, preparation liquefaction thing; In heating, stir, the speed of stirring can be according to the size setting of inventory and agitated reactor; 2) after timber liquefied matter is reduced to room temperature, to the synthetics hexamethylenetetramine that wherein adds 4-6% timber liquefied matter weight, behind the 1h; Be heated to 160-175 ℃ and obtain spinning solution; Subsequently spinning solution is placed spinning machine, when spinning solution was heated to 110-130 ℃, (melt spinning) can reel off raw silk from cocoons; The fiber that obtains synthesizing, the rotating speed of receiving roll dies can be provided with according to wire vent speed voluntarily; 3) synthetic fiber being placed volume ratio is 1: 1 the formaldehyde and the mixed liquor of hydrochloric acid, is heated to 85-95 ℃, and insulation 2-4h reduces to room temperature after washing drying, obtains precursor; 4) precursor is placed activating apparatus, carry out " one-step method " physically activated, under nitrogen protection, be heated to 700-900 ℃, precursor and activator are reacted, promptly get wooden activated carbon fiber.
Preferably, in the preceding method, temperature retention time is 2.5h in the step 1).
Preferably, in the preceding method, the acid catalyst that uses in the step 1) is the phosphoric acid or the sulfuric acid of 0.4-0.6 times of wood powder weight.
Preferably, in the preceding method, the heating rate when heating in the step 3) is 10 ℃/h.
Preferably, in the preceding method, the heating rate when heating in the step 4) is 2-4 ℃/min.
Preferably, in the preceding method, the activator that uses in the step 4) is steam, and flow is 1.0-2.5ml/min/g, and the time that feeds steam is 10-90min.
Preferably, in the preceding method, after stopping in the step 4) feeding steam, activating apparatus is lowered the temperature automatically, treat that temperature stops to feed nitrogen when reducing to 300-350 ℃.
Preferably, in the preceding method, the wood powder in the step 1) is that wood machining residues is pulverized, the 30-80 order wood powder that screening obtains.
Adopt the performance indications of wooden activated carbon fiber of " one-step method " of the present invention physically activated preparation following:
Yield of activation: 10.45-48.75 (%)
Specific area: 740.50-2641.085 (m
2/ g)
Micropore specific area: 449.176-2092.531 (m
2/ g)
Total pore volume: 0.353-1.388 (cm
3/ g)
Micropore pore volume: 0.190-0.898 (cm
3/ g)
Average pore size: 0.900-1.279 (nm)
The invention has the advantages that:
(1) the present invention is raw material with the wood machining residues; Belong to living beings, compare with prior biological matter carbon fiber (for example viscose glue base, lignin-base), maximum advantage is from living beings, to extract chemical compositions such as cellulose and lignin separately; But all utilize; Simplify production technology, reduced production cost, increased the utilization rate of living beings.
(2) compare with the chemical activation technology of activated carbon fiber, its mainly with highly basic that activating apparatus is had severe corrosive as activator, the present invention adopts steam as activator, environmental pollution is little, and is little to corrosion of equipment property, helps sustainable development.
(3) the present invention adopts " one-step method " physically activated preparing product, can reduce the energy resource consumption in the preparation process, has simplified the input of processing step and production equipment, has improved the product yield.
(4) the wooden activated carbon fiber of the present invention's preparation is superior to other industrialization activated carbon fibers in performance, and for example the specific area of viscose glue base, the fine base of polypropylene, phenolic aldehyde base and asphalt activity carbon fiber is respectively 1000-1500m
2/ g, 700-1200m
2/ g, 1000-2300m
2/ g and 1000-2000m
2/ g, and the specific area of the active wooden carbon fiber that employing the inventive method makes is 740.50-2641.085m
2/ g.
Description of drawings
Fig. 1 is the process chart of the active wooden carbon fiber of preparation in the embodiment of the invention 1~6.
The specific embodiment
Following examples are used to explain the present invention, but are not used for limiting scope of the present invention.If do not specialize the conventional means that used technological means is well known to those skilled in the art among the embodiment, the raw materials used commercial goods that is.
The preparation of embodiment 1 active wooden carbon fiber
As shown in Figure 1, wood machining residues is ground into 30 orders after, put in the middle of the liquefying plant.Add the phenol of 4 times of wood powder weight and the phosphoric acid of 0.4 times of wood powder weight again, mixture heated to 160 ℃, insulation 2.5h.After timber liquefied matter is reduced to room temperature, add the hexamethylenetetramine of 4% liquefaction thing weight, through 1 hour, be warmed up to 170 ℃, synthetic spinning solution.Subsequently spinning solution is placed spinning machine, when spinning solution is heated to 120 ℃, receive silk with the speed of receiving 100 rev/mins of roll dies.It is 1: 1 formaldehyde and the mixed liquor of hydrochloric acid that synthetic fiber is placed volume ratio, is heated to 85 ℃ with the heating rate of 10 ℃/h, is incubated 2h.It is dry to wait to reduce to the room temperature after washing.The precursor that takes by weighing 2.85g places activation furnace; Under protection of nitrogen gas, will be warmed up to 800 ℃ with the speed of 3 ℃/min after, feed steam in the time of insulation; Flow is 1ml/min/g; And behind 60min, close the steam generator, and activation furnace is lowered the temperature automatically,, temperature stops to feed nitrogen when reaching 350 ℃.
The yield of activation of the activated carbon fiber of preparation is 40.702%, specific area 1249.511m
2/ g, micropore specific area are 968.492m
2/ g, total pore volume is 0.644cm
3/ g, micropore pore volume are 0.384cm
3/ g, average pore size is 1.031nm.
The preparation of embodiment 2 active wooden carbon fibers
After wood machining residues is ground into 60 orders, put in the middle of the liquefying plant.Add the phenol of 5 times of wood powder weight and the phosphoric acid of 0.5 times of wood powder weight again, mixture heated to 160 ℃, insulation 2.5h.After timber liquefied matter is reduced to room temperature, add the hexamethylenetetramine of liquefaction thing 5% weight, through 1 hour, be warmed up to 170 ℃, synthetic spinning solution.Subsequently spinning solution is placed spinning machine, when spinning solution is heated to 120 ℃, receive silk with the speed of receiving 100 rev/mins of roll dies.It is 1: 1 formaldehyde and the mixed liquor of hydrochloric acid that synthetic fiber is placed volume ratio, is heated to 85 ℃ with the heating rate of 10 ℃/h, is incubated 2h.It is dry to wait to reduce to the room temperature after washing.The precursor that takes by weighing 4.49g places activation furnace, under protection of nitrogen gas, will be warmed up to 800 ℃ with the speed of 3 ℃/min after; Feed steam in the time of insulation; Its flow is 1.5ml/min/g, and behind 90min, closes the steam generator, and activation furnace is lowered the temperature automatically., temperature stops to feed nitrogen when reaching 300 ℃.
The yield of activation of the activated carbon fiber of preparation is 28.721%, specific area 1737.839m
2/ g, micropore specific area are 1388.637m
2/ g, total pore volume is 0.899cm
3/ g, micropore pore volume are 0.556cm
3/ g, average pore size is 1.035nm.
The preparation of embodiment 3 active wooden carbon fibers
After wood machining residues is ground into 80 orders, put in the middle of the liquefying plant.Add the phenol of 5 times of wood powder weight and the sulfuric acid of 0.6 times of wood powder weight again, mixture heated to 160 ℃, insulation 2.5h.After timber liquefied matter is reduced to room temperature, add the hexamethylenetetramine of liquefaction thing 6% weight, through 1 hour, be warmed up to 170 ℃, synthetic spinning solution.Subsequently spinning solution is placed spinning machine, when spinning solution is heated to 120 ℃, receive silk with the speed of receiving 100 rev/mins of roll dies.It is 1: 1 formaldehyde and the mixed liquor of hydrochloric acid that synthetic fiber is placed volume ratio, is heated to 85 ℃ with the heating rate of 10 ℃/h, is incubated 2h.It is dry to wait to reduce to the room temperature after washing.The precursor that takes by weighing 4.49g places activation furnace, under protection of nitrogen gas, will be warmed up to 800 ℃ with the speed of 2 ℃/min after; Feed steam in the time of insulation; Its flow is 1.0ml/min/g, and behind 60min, closes the steam generator, and activation furnace is lowered the temperature automatically., temperature stops to feed nitrogen when reaching 320 ℃.
The yield of activation of the activated carbon fiber of preparation is 43.371%, specific area 1113.907m
2/ g, micropore specific area are 897.051m
2/ g, total pore volume is 0.572cm
3/ g, micropore pore volume are 0.358cm
3/ g, average pore size is 1.028nm.
The preparation of embodiment 4 active wooden carbon fibers
After wood machining residues is ground into 60 orders, put in the middle of the liquefying plant.Add the phenol of 5 times of wood powder weight and the phosphoric acid of 0.5 times of wood powder weight again, mixture heated to 150 ℃, insulation 2.5h.After timber liquefied matter is reduced to room temperature, add the hexamethylenetetramine of liquefaction thing 6% weight, through 1 hour, be warmed up to 175 ℃, synthetic spinning solution.Subsequently spinning solution is placed spinning machine, when spinning solution is heated to 120 ℃, receive silk with the speed of receiving 100 rev/mins of roll dies.It is 1: 1 formaldehyde and the mixed liquor of hydrochloric acid that synthetic fiber is placed volume ratio, is heated to 85 ℃ with the heating rate of 10 ℃/h, is incubated 2h.It is dry to wait to reduce to the room temperature after washing.The precursor that takes by weighing 4.31g places activation furnace, under protection of nitrogen gas, will be warmed up to 900 ℃ with the speed of 3 ℃/min after; Feed steam in the time of insulation; Its flow is 1.0ml/min/g, and behind 60min, closes the steam generator, and activation furnace is lowered the temperature automatically., temperature stops to feed nitrogen when reaching 350 ℃.
The yield of activation of the activated carbon fiber of preparation is 10.451%, specific area 2641.085m
2/ g, micropore specific area are 2029.531m
2/ g, total pore volume is 1.388cm
3/ g, micropore pore volume are 0.898cm
3/ g, average pore size is 1.051nm.
The preparation of embodiment 5 active wooden carbon fibers
After wood machining residues is ground into 80 orders, put in the middle of the liquefying plant.Add the phenol of 5 times of wood powder weight and the phosphoric acid of 0.6 times of wood powder weight again, mixture heated to 160 ℃, insulation 2.5h.After timber liquefied matter is reduced to room temperature, add the hexamethylenetetramine of liquefaction thing 6% weight, through 1 hour, be warmed up to 170 ℃, synthetic spinning solution.Subsequently spinning solution is placed spinning machine, when spinning solution is heated to 120 ℃, receive silk with the speed of receiving 100 rev/mins of roll dies.It is 1: 1 formaldehyde and the mixed liquor of hydrochloric acid that synthetic fiber is placed volume ratio, is heated to 85 ℃ with the heating rate of 10 ℃/h, is incubated 2h.It is dry to wait to reduce to the room temperature after washing.The precursor that takes by weighing 3.0g places activation furnace, under protection of nitrogen gas, will be warmed up to 700 ℃ with the speed of 2 ℃/min after; Feed steam in the time of insulation; Its flow is 1.0ml/min/g, and behind 60min, closes the steam generator, and activation furnace is lowered the temperature automatically., temperature stops to feed nitrogen when reaching 350 ℃.
The yield of activation of the activated carbon fiber of preparation is 48.750%, specific area 784.370m
2/ g, micropore specific area are 692.009m
2/ g, total pore volume is 0.353cm
3/ g, micropore pore volume are 0.269cm
3/ g, average pore size is 0.89981nm.
The preparation of embodiment 6 active wooden carbon fibers
After wood machining residues is ground into 80 orders, put in the middle of the liquefying plant.Add the phenol of 5 times of wood powder weight and the phosphoric acid of 0.6 times of wood powder weight again, mixture heated to 160 ℃, insulation 2.5h.After timber liquefied matter is reduced to room temperature, add the hexamethylenetetramine of liquefaction thing 5% weight, through 1 hour, be warmed up to 165 ℃, synthetic spinning solution.Subsequently spinning solution is placed spinning machine, when spinning solution is heated to 120 ℃, receive silk with the speed of receiving 100 rev/mins of roll dies.It is 1: 1 formaldehyde and the mixed liquor of hydrochloric acid that synthetic fiber is placed volume ratio, is heated to 90 ℃ with the heating rate of 10 ℃/h, is incubated 2h.It is dry to wait to reduce to the room temperature after washing.The precursor that takes by weighing 4.49g places activation furnace, under protection of nitrogen gas, will be warmed up to 800 ℃ with the speed of 4 ℃/min after; Feed steam in the time of insulation; Its flow is 1.0ml/min/g, and behind 60min, closes the steam generator, and activation furnace is lowered the temperature automatically., temperature stops to feed nitrogen when reaching 350 ℃.
The yield of activation of the activated carbon fiber of preparation is 39.986%, specific area 1262.962m
2/ g, micropore specific area are 965.120m
2/ g, total pore volume is 0.680cm
3/ g, micropore pore volume are 0.385cm
3/ g, average pore size is 1.076nm.
Fig. 1 is the process chart of the active wooden carbon fiber of preparation among the embodiment 1~6.
Though, the present invention has been done detailed description in the preceding text with general explanation and specific embodiments, on basis of the present invention, can to some modifications of do or improvement, this will be apparent to those skilled in the art.Therefore, these modifications or the improvement on the basis of not departing from spirit of the present invention, made all belong to the scope that requirement of the present invention is protected.
Claims (7)
1. the preparation method of the wooden carbon fiber of activity is characterized in that, may further comprise the steps:
1) phenol of 4-6 times of wood powder weight of adding in wood powder in the presence of acid catalyst, is heated to 150-160 ℃, insulation, preparation liquefaction thing;
2) hexamethylenetetramine of adding 4-6% liquefaction thing weight in the liquefaction thing is heated to 160-175 ℃ and obtains spinning solution, melt spinning when the spinning solution temperature reaches 110-130 ℃, the fiber that obtains synthesizing;
3) synthetic fiber being placed volume ratio is 1: 1 the formaldehyde and the mixed liquor of hydrochloric acid, is heated to 85-95 ℃, and insulation 2-4h reduces to room temperature after washing drying, obtains precursor;
4) under nitrogen protection, be heated to 700-900 ℃, precursor and activator are reacted, promptly get wooden activated carbon fiber.
2. preparation method according to claim 1 is characterized in that, temperature retention time is 2.5h in the step 1).
3. preparation method according to claim 1 is characterized in that, the acid catalyst that uses in the step 1) is the phosphoric acid or the sulfuric acid of 0.4-0.6 times of wood powder weight.
4. preparation method according to claim 1 is characterized in that, the heating rate when heating in the step 3) is 10 ℃/h.
5. preparation method according to claim 1 is characterized in that, the heating rate when heating in the step 4) is 2-4 ℃/min.
6. according to each described preparation method of claim 1-5, it is characterized in that the activator that uses in the step 4) is steam, flow is 1.0-2.5ml/min/g, and the time that feeds steam is 10-90min.
7. according to each described preparation method of claim 1-5, it is characterized in that the wood powder in the step 1) is that wood machining residues is pulverized, the 30-80 order wood powder that screening obtains.
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CN102817112A (en) * | 2012-09-11 | 2012-12-12 | 长春高琦聚酰亚胺材料有限公司 | Preparation method of activated carbon fibers |
CN103290526A (en) * | 2013-06-03 | 2013-09-11 | 北京林业大学 | Preparation method for wood active carbon fiber |
CN103397404A (en) * | 2013-07-15 | 2013-11-20 | 北京林业大学 | Method for increasing specific surface area of wooden active carbon fiber |
CN103451920A (en) * | 2013-08-16 | 2013-12-18 | 北京林业大学 | Preparation method of silver-loaded active wood carbon fiber |
CN103469368A (en) * | 2013-09-06 | 2013-12-25 | 北京林业大学 | Wood carbon fiber precursor and preparation method thereof |
CN103774285A (en) * | 2013-12-31 | 2014-05-07 | 北京梦狐宇通竹纤维研究开发中心 | Preparation method for cellulose active carbon nanofibre adsorbing material |
CN105040162A (en) * | 2015-06-11 | 2015-11-11 | 天津科技大学 | Woody hollow fibers and preparation method of woody hollow active carbon fibers |
CN105220275A (en) * | 2014-06-13 | 2016-01-06 | 北京昆仑江海科技发展有限公司 | A kind of preparation method of cellulose base activated carbon fiber |
CN105274656A (en) * | 2015-10-20 | 2016-01-27 | 天津科技大学 | Wood mesoporous activated carbon precursor and preparation method thereof |
CN105293488A (en) * | 2015-10-23 | 2016-02-03 | 北京林业大学 | Lignin-based activated carbon microsphere and preparation method and application thereof |
CN105803583A (en) * | 2016-05-12 | 2016-07-27 | 安徽金叶碳素科技有限公司 | Rare earth carbon powder and preparation method thereof |
CN105949414A (en) * | 2016-05-12 | 2016-09-21 | 安徽金叶碳素科技有限公司 | Superhard carbon powder and preparation method thereof |
CN106019870A (en) * | 2016-06-07 | 2016-10-12 | 上海活性炭厂有限公司 | Environment-friendly carbon powder and preparation method thereof |
CN108330569A (en) * | 2018-02-08 | 2018-07-27 | 北京林业大学 | A kind of lignin-base activated carbon fiber presoma and the preparation method and application thereof |
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 |
CN115467050A (en) * | 2022-08-25 | 2022-12-13 | 广西大学 | Preparation method of boron-modified wood liquefied carbon fiber spinning solution |
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CN105274656A (en) * | 2015-10-20 | 2016-01-27 | 天津科技大学 | Wood mesoporous activated carbon precursor and preparation method thereof |
CN105274656B (en) * | 2015-10-20 | 2017-07-04 | 天津科技大学 | A kind of preparation method of wooden mesopore activated carbon precursor and fiber |
CN105293488A (en) * | 2015-10-23 | 2016-02-03 | 北京林业大学 | Lignin-based activated carbon microsphere and preparation method and application thereof |
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CN106019870A (en) * | 2016-06-07 | 2016-10-12 | 上海活性炭厂有限公司 | Environment-friendly carbon powder and preparation method thereof |
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CN115467050A (en) * | 2022-08-25 | 2022-12-13 | 广西大学 | Preparation method of boron-modified wood liquefied carbon fiber spinning solution |
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