CN105040162A - Woody hollow fibers and preparation method of woody hollow active carbon fibers - Google Patents
Woody hollow fibers and preparation method of woody hollow active carbon fibers Download PDFInfo
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Abstract
The invention provides woody hollow fibers and a preparation method of woody hollow active carbon fibers. With biomass resources such as wood as raw materials, a raw material liquefaction spinning solution is spun to obtain as-spun fibers, the as-spun fibers are prepared into the hollow fibers through a dissolving-curing process, and then the hollow fibers are prepared into the woody hollow active carbon fibers through carbonizing and activating processes. Through the method, the biomass resources are taken as the main raw materials of the active carbon fibers, so that the production cost of the hollow active carbon fibers is lowered, the utilization rate of the biomass resources and the additional value of the fibers are improved, and the industrial production of the woody hollow active carbon fibers is facilitated. The specific surface area of the hollow active carbon fibers is 1350-2854m<2>/g, and the hollow ratio of the hollow active carbon fibers is 40%-90%. A wood liquefaction hollow dissolving agent is low in cost, excellent in quality, simple in process and free of secondary pollution. Meanwhile, with the biomass resources as the raw materials of the hollow active carbon fibers, the production cost is lowered, and the competitiveness is high.
Description
Technical field
The invention provides the preparation method of a kind of wooden doughnut and wooden hollow activated carbon fiber, specifically, that one utilizes the biomass resource liquefied substances such as timber to prepare hollow activated carbon fiber, the invention still further relates to for the preparation of hollow activated carbon fiber lytic agent used, and the hole control technique in activation process.
Background technology
Hollow activated carbon fiber is a kind of activated carbon fiber with hollow structure.Hollow activated carbon fiber remains the structure of hollow precursor.Hollow activated carbon fiber inside has hollow structure, and internal diameter is generally between 20-100 μm, and wall thickness is the 1/4-1/10 of internal diameter.The finger-like porous layer be connected with top layer, loose structure plays the effect of support.Wall all has nanometer level microporous, micropore distribution is abundant.Pore-size distribution is narrow, the atomic hole rich content of below 1nm.A large amount of micropore is directly opened on fiber surface, and Small molecular adsorbate is easily entered.Therefore be a kind of good sorbing material.Because it has the structure of hollow, the total specific area specific activity Carbon fibe of inside and outside wall is much bigger, in addition abundant micropore, and therefore the absorption property specific activity Carbon fibe of hollow activated carbon fiber wants large many.
Hollow activated carbon fiber owing to having higher heat and chemical stability and mechanical strength than traditional polymer film, the application prospect making it in fields such as food industry, environmental project, electronics industry, petrochemical industry, chemical industry, have it more wide in high temperature, high pressure, strong acid, highly basic or organic solvent system especially.At present, hollow activated carbon fiber is more for gas separaion, although hollow activated carbon fiber is all not too high to gas separation coefficient, has much higher separation rate than common organic film and inoranic membrane.In addition, it is good that hollow activated carbon fiber also has chemical stability, the advantage that can at high temperature use.The instructions for use that some is harsh especially can be met, the fields such as high-temperature gas separation, acid-base material separation can be used for.
Current hollow activated carbon fiber is main mainly with polypropylene fine hollow activated carbon fiber.Along with day by day strengthening of people's environmental consciousness and petering out of fossil resource, for the negative effect of reply fossil resource exploitation to ball ecological environment, reduce activated carbon fiber to the dependence of fossil resource raw material, Wooden Biomass hollow activated carbon fiber also becomes the emphasis of research and development.
Summary of the invention
The present inventor for raw material with biomass resources such as timber, utilizes its liquefied spinning liquid to be spun into as-spun fibre, by dissolving-curing process, protofilament is prepared into doughnut, be prepared into wooden hollow activated carbon fiber through series of process such as charing, activation.The method, using biomass resource as the main raw material of activated carbon fiber, reduces the production cost of hollow activated carbon fiber, improves biomass resource utilization rate and value-added content of product, is conducive to the suitability for industrialized production of wooden hollow activated carbon fiber.
The object of this invention is to provide a kind of method utilizing the biomass liquefying things such as timber to prepare hollow activated carbon fiber.
First the biological materials such as timber are synthesized spinning solution through post liquefaction by the present invention, and the as-spun fibre of spinning is dissolved into wooden doughnut through lytic agent, carbonize, activate acquisition hollow activated carbon fiber after regelate.
Therefore, another object of the present invention is to provide a kind of lytic agent that can be used for manufacturing a large amount of wooden doughnut.
Object of the present invention also comprises the hole regulate and control method providing and prepare above-mentioned wooden hollow activated carbon fiber.
Wooden doughnut of the present invention, prepared by following method:
1) biomass material is ground into powder, adds 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 Wood liquefied spinning liquid;
3) Wood liquefied spinning liquid is spun into as-spun fibre;
4) as-spun fibre immerses in the acid solution of aldehyde, is heated to 60 ~ 90 DEG C with the programming rate of 10 ~ 30 DEG C/h, then at 60 ~ 90 DEG C of solidification 1h;
5), after cured fiber washing totally, immerse 50 DEG C of dissolving 10-30min in lytic agent and obtain doughnuts;
6) doughnut is immersed concentration be respectively 18.5% formaldehyde and 18.5% hydrochloric acid composition mass percent the aqueous solution in, be heated to 90 DEG C with the programming rate of 10 DEG C/h, carry out regelate and obtain wooden doughnut.
Wherein, described biomass material can be timber, bamboo wood, stalk, string etc.
Wherein, the fineness of described biomass material powder is 20 ~ 80 orders.
Wherein, described step 1) be: the biomass materials such as timber are ground into powder, add the phenol of raw material weight 4 ~ 6 times and be equivalent to the phosphoric acid catalyst that phenol adds 6% ~ 8% of weight, stirring at ambient pressure in 150 DEG C ~ 160 DEG C reaction 2.5 ~ 3h, obtain liquefied substance.
Wherein, described synthetics is selected from the one in paraformaldehyde, furfural, hexamethylenetetramine, metaformaldehyde.
Wherein, the acid solution of described aldehyde is the oxalic acid solution of formaldehyde or the hydrochloric acid solution of formaldehyde.
Wherein, the acid solution of described aldehyde be containing concentration of formaldehyde be 18.5%, concentration of hydrochloric acid is the solution of 18.5%.
Lytic agent of the present invention is acetone or the methanol solution of concentration 30 ~ 50%.
Wooden hollow activated carbon fiber of the present invention, prepared by following method:
Wooden doughnut 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 the wooden hollow activated carbon fiber of different absorption property.
Hollow activated carbon fiber prepared by the inventive method, has following characteristics:
Specific area: 1350 ~ 2854 (m
2/ g),
Hollow rate: 40 ~ 90 (%),
Yield: 15 ~ 40 (%)
Average pore size: 1.05 ~ 1.51 (nm).
Beneficial effect
The present inventor is according to the characteristic of biological material, and application liquefaction technology and dissolving-curing technology, through large quantity research and test, adopt the Novel hollow activated carbon fiber that the technology of the present invention utilizes biological material liquefied substance to prepare, its hollow rate can reach 40 ~ 90%.In addition, this invention utilizes the wooden liquefied substance hollow lytic agent of preparation, has of high quality and at a reasonable price, and technique is simple, non-secondary pollution, and suitability for industrialized production is convenient.Meanwhile, this technology, using biomass resource as hollow activated carbon fiber raw material, reduces production cost, commercially has very strong competitiveness.
Detailed description of the invention
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.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.Spinning solution is added in spinning machine, at 0.05MPaN
2depress and be spun into timber liquefied matter as-spun fibre at 120 DEG C.
As-spun fibre 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 80 DEG C with the programming rate of 10 DEG C/h, then process 1h 80 DEG C of solidifications.After cured fiber washing is clean, immerses 50 DEG C of dissolving 10min in the acetone solution agent of 30% and obtain doughnut.
Doughnut is immersed again by concentration be respectively 18.5% formaldehyde and 18.5% the aqueous solution of mass percent that forms of hydrochloric acid in, be heated to 90 DEG C with the programming rate of 10 DEG C/h, then obtain wooden hollow precursor at 90 DEG C of solidification process 4h.
Wooden hollow precursor 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 hollow activated carbon fiber.
The specific area prepared: 2048m
2/ g; Hollow rate: 68%; Yield: 25%.
Embodiment 2
Mao bamboon is ground into 60 object powder, be then 6% of phenol addition by the phenol of 5 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.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.
As-spun fibre 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 90 DEG C with the programming rate of 20 DEG C/h, then process 1h 90 DEG C of solidifications.After cured fiber washing is clean, immerses 50 DEG C of dissolving 30min in the methyl alcohol lytic agent of 50% and obtain doughnut.Doughnut is immersed again by concentration be respectively 18.5% formaldehyde and 18.5% the aqueous solution of mass percent that forms of hydrochloric acid in, be heated to 90 DEG C with the programming rate of 10 DEG C/h, then obtain wooden hollow precursor at 90 DEG C of solidification process 4h.
Wooden hollow precursor 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 2 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.
The specific area prepared: 2854m
2/ g; Hollow rate: 90%; Yield: 15%.
Embodiment 3
Cotton stalk is ground into 40 object powder, be then 8% of phenol addition by the phenol of 6 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.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.
As-spun fibre 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 60 DEG C with the programming rate of 30 DEG C/h, then process 1h 60 DEG C of solidifications.After cured fiber washing is clean, immerses 50 DEG C of dissolving 20min in the methyl alcohol lytic agent of 40% and obtain doughnut.Doughnut is immersed again by concentration be respectively 18.5% formaldehyde and 18.5% the aqueous solution of mass percent that forms of hydrochloric acid in, be heated to 90 DEG C with the programming rate of 10 DEG C/h, then obtain wooden hollow precursor at 90 DEG C of solidification process 4h.
Wooden hollow precursor is put into retort, at N
2(N under protection
2flow is 100mL/min) be uniformly heated to 750 DEG C with the programming rate of 2 DEG C/min, after charing 30min, logical 6g/min steam carries out activation processing 60min then cool to room temperature, obtains wooden center hole activated carbon fiber.
The specific area prepared: 1350m
2/ g; Hollow rate: 40%; Yield: 40%.
Embodiment 4
Chinese white poplar is ground into 20 object powder, be then 6% of phenol addition by the phenol of 6 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.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.
As-spun fibre 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 70 DEG C with the programming rate of 25 DEG C/h, then process 1h 70 DEG C of solidifications.After cured fiber washing is clean, immerses 50 DEG C of dissolving 30min in the methyl alcohol lytic agent of 50% and obtain doughnut.Doughnut is immersed again by concentration be respectively 18.5% formaldehyde and 18.5% the aqueous solution of mass percent that forms of hydrochloric acid in, be heated to 90 DEG C with the programming rate of 10 DEG C/h, then obtain wooden hollow precursor at 90 DEG C of solidification process 4h.
Wooden hollow precursor is put into retort, at N
2(N under protection
2flow is 100mL/min) be uniformly heated to 700 DEG C with the programming rate of 2 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.
The specific area prepared: 1967m
2/ g; Hollow rate: 54%; Yield: 36%.
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 (9)
1. the preparation method of a wooden doughnut; It is characterized in that step is as follows:
1) biomass material is ground into powder, adds 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, obtain Wood liquefied spinning liquid;
3) Wood liquefied spinning liquid is spun into as-spun fibre;
4) as-spun fibre immerses in the acid solution of aldehyde, is heated to 60 ~ 90 DEG C with the programming rate of 10 ~ 30 DEG C/h, then at 60 ~ 90 DEG C of solidification 1h;
5), after cured fiber washing totally, immerse 50 DEG C of dissolving 10-30min in lytic agent and obtain doughnuts;
6) doughnut is immersed concentration be respectively 18.5% formaldehyde and 18.5% hydrochloric acid composition mass percent the aqueous solution in, be heated to 90 DEG C with the programming rate of 10 DEG C/h, carry out regelate and obtain wooden doughnut.
2. the method for claim 1, is characterized in that described biomass material is one or more of timber, bamboo wood, stalk or string.
3. the method for claim 1, is characterized in that the fineness of described biomass material powder is 20 ~ 80 orders.
4. the method for claim 1, it is characterized in that described step 1) be: biomass material is ground into powder, add the phenol of raw material weight 4 ~ 6 times and be equivalent to the phosphoric acid catalyst that phenol adds 6% ~ 8% of weight, stir at ambient pressure in 150 DEG C ~ 160 DEG C reaction 2.5 ~ 3h, obtain liquefied substance.
5. method as claimed in claim 4, is characterized in that described synthetics is selected from the one in paraformaldehyde, furfural, hexamethylenetetramine, metaformaldehyde.
6. the method for claim 1, is characterized in that described step 4) in, the acid solution of aldehyde is the oxalic acid solution of formaldehyde or the hydrochloric acid solution of formaldehyde.
7. method as claimed in claim 6, it is characterized in that the hydrochloric acid solution of described formaldehyde be containing concentration of formaldehyde be 18.5%, concentration of hydrochloric acid is the solution of 18.5%.
8. the method for claim 1, is characterized in that described step 5) in lytic agent be acetone or the methanol solution of concentration 30 ~ 50%.
9. utilize the wooden doughnut of claim 1 to prepare the method for wooden hollow activated carbon fiber, it is characterized in that: wooden doughnut is put into retort, at N
2under protection, 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 hollow activated carbon fiber.
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| CN105536729A (en) * | 2015-12-11 | 2016-05-04 | 苏州贝多环保技术有限公司 | Adsorption material and preparation method thereof |
| CN105536731A (en) * | 2015-12-11 | 2016-05-04 | 苏州贝多环保技术有限公司 | Composite adsorption material and preparation method thereof |
| CN105568413A (en) * | 2015-12-22 | 2016-05-11 | 中国科学院山西煤炭化学研究所 | Lignin-based hollow fiber and preparation method thereof |
| WO2017089585A1 (en) * | 2015-11-25 | 2017-06-01 | Deutsche Institute Für Textil- Und Faserforschung Denkendorf | Method for producing a lignin-based composition |
| CN109385889A (en) * | 2018-11-08 | 2019-02-26 | 珠海鑫康源新材料科技有限公司 | A kind of Anti-bacterial radiation-proof fabric |
| 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 |
| CN114250531A (en) * | 2021-12-21 | 2022-03-29 | 青岛华世洁环保科技有限公司 | Preparation method of activated carbon fiber and activated carbon fiber prepared by same |
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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 |
| CN114250531A (en) * | 2021-12-21 | 2022-03-29 | 青岛华世洁环保科技有限公司 | Preparation method of activated carbon fiber and activated carbon fiber prepared by same |
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