CN109137139A - A kind of preparation method of lignin-base fiber - Google Patents
A kind of preparation method of lignin-base fiber Download PDFInfo
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- CN109137139A CN109137139A CN201810842740.8A CN201810842740A CN109137139A CN 109137139 A CN109137139 A CN 109137139A CN 201810842740 A CN201810842740 A CN 201810842740A CN 109137139 A CN109137139 A CN 109137139A
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- Prior art keywords
- alkali lignin
- spinning
- powder
- base fiber
- preparation
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
Abstract
The present invention provides a kind of preparation method of alkali lignin base fiber with small diameter, comprising the following steps: (1) is precipitated from black paper-making liquid of alkali pulping using sulfuric acid and isolated alkali lignin powder；(2) alkali lignin powder and polyethylene glycol are dissolved in dimethyl formamide solution in a heated condition, obtain the spinning solution for preparing alkali lignin base fiber；(3) spinning solution is added in spin duct, using centrifugal spinning method, adjusts spinning revolving speed, obtain alkali lignin base fiber.Processing mode through the invention, resulting alkali lignin base fiber have small diameter, and the later period is further carbonized and activation processing can be made into lignin-base nano carbon fibre, can be widely applied to the fields such as environmental protection, electronics, medical sanitary, chemical industry.Also, method of the invention is easy to operate, and less energy consumption, time-consuming are short, high-efficient, has preferable prospects for commercial application.
Description
Technical field
The invention belongs to the fields of the manufacture of fiber, and in particular to a kind of to have small diameter using plant material preparation
The method of fiber.
Background technique
As third generation adsorption functional material, activated carbon fiber be it is a kind of there is porous carbon fibre material, have than
Surface area is big, aperture is moderate and is evenly distributed, the advantages that adsorption rate is fast, impurity is few, can be widely applied to Water warfare, air
Purification, organic solvent recycling, aviation, military affairs, food, catalyst carrier, electrode material etc..The raw material master of activated carbon fiber
It will be from glutinous glue based fibre, phenolic aldehyde base fiber, pan based fibers and pitch-based fiber.But with fossil resource
It is increasingly in short supply and they exploitation and use process in caused by environmental disruption and pollution problem so that activated carbon fiber is not
With sustainable developability, this also results in the extensive attention of researchers.Highly advocating environmentally protective, energy-saving and emission-reduction the presents
How it, be raw material and be used to prepare using from a wealth of sources, cheap, environmentally protective biomass resource substitution fossil resource
Activated carbon fiber becomes an important topic.
Lignin and cellulose and hemicellulose etc. constitute plant skeleton, and the storage in natural plant body is very rich
Richness is only second to cellulose.Every year, from up to 50,000,000 tons/year of lignin in industrial pulp and paper making discharge black liquor, and had
Imitate 5% of amount less than total amount that utilizes, remainder is discharged discarded or burning and obtains energy, cause certain environmental pollution with
The wasting of resources.Using lignin as raw material, and high-valued processing is prepared into the functional materials such as activated carbon fiber, not only can achieve change
Waste be changed into values and realizes the purpose of the sustainability of activated carbon fiber raw material, but also can be to avoid polluting the environment and break
It is bad.
In lignin-base activated carbon fiber preparation process, powdered lignin spinning moulding be fiber be it is most important and
One of the step of being most difficult to.In existing lignin-base fiber spinning processes, wet spinning, dry spinning, melt spinning and quiet
Electrical spinning method is the main method by lignin conversion for fiber.But prepared by wet spinning, dry spinning, melt spinning
Obtained lignin-base fibre diameter is relatively large, and mostly 20 μm or more, some is even higher than 50 μm.It is straight in order to reduce fiber
Diameter improves the specific surface area and absorption property of final activated carbon fiber, and electrospinning process is becoming increasingly popular, but the method obtains
Though the diameter of lignin-base fiber reduced, still have 5 μm or so, and electrostatic spinning process need higher voltage and
Lower concentration of dope, this not only adds risk to also improve preparation cost.Therefore, in order to further decrease lignin
Base fibre diameter reduces energy consumption, to prepare there is the activated carbon fiber of high-specific surface area to provide basic raw material, there is an urgent need to one
Kind can obtain the lesser preparation method of lignin-base fibre diameter.
Summary of the invention
This field there are aiming at the problem that, the purpose of the present invention is to provide a kind of alkali lignin base with small diameter
The preparation method of fiber.
Another object of the present invention is to provide a kind of lignin-base activity carbon fibers that can be prepared into bigger serface
The raw material of dimension, i.e. lignin-base fiber.
The present invention to solve problems of the prior art, and then proposes a kind of alkali lignin base with small diameter
The preparation method of fiber, comprising the following steps: Step 1: black liquor powder is mixed with water, filtered after mixing evenly using filter paper,
To remove larger particles insoluble matter in black liquor；It takes filtrate that sulfuric acid is gradually added to be precipitated, be centrifugated using low speed centrifuge
It is precipitated, alkali lignin powder will be obtained after the drying of gained pellet frozen；Walk poly- two, by alkali lignin powder and polyethylene glycol
It is dissolved in dimethyl formamide solution in proportion in a heated condition, obtains the spinning solution for preparing alkali lignin base fiber；Step
Rapid three, spinning solution is added in spin duct, using centrifugal spinning method, adjusts spinning revolving speed, obtain alkali lignin base fiber.
Further, alkali lignin powder is the lignin isolated from pulping and paper-making waste liquid in the step poly- one, true
After sky is dry, grinding is carefully to more than 100 mesh.
Further, in the step 2, the molecular weight of polyethylene glycol is 100K-600K.
Further, the polyethylene glycol quality in the step 2 is the quality based on alkali lignin powder, and ratio is
0.5%-10%.
Further, the alkali lignin powder Yu polyethylene glycol of the step 2 are dissolved in the matter in dimethyl formamide solution
Amount score is 5%-70%.
Further, the alkali lignin powder and polyethylene glycol are dissolved into dimethyl formamide solution, first that alkali is wooden
The sequence that plain powder is slowly added to add both polyethylene glycol, or addition in the solution with magnetic agitation is exchanged also
It can.
Further, the heating condition of the step 2, both alkali lignin powder and polyethylene glycol are in dimethylformamide
Heating temperature when dissolving in solution is 25 DEG C -85 DEG C.
Further, the spin duct revolving speed of the centrifugal box-spinning machine of the step 3 is that 3000 turns/min-20000 turns/min, is spun
Fiber tube filament mouth is 10cm-70cm away from the distance for receiving filament plate.
Further, spinning solution is first fitted into spin duct by the spin duct in spinning, and logical screw thread, which is tightened and is fixed on, to be turned
On son, and guarantee turns on the switch spin duct after starting rotation and does not loosen, and fixes spin duct filament mouth not at a distance from receipts filament plate
Become.
Further, during poly- three centrifugal spinning of the step, whole environment temperature control is at 25 DEG C -35 DEG C, environment phase
It is 20-80RH% to humidity.
The lignin-base fiber that the method for the present invention is prepared is also within the scope of the present invention.
By many experiments, in conjunction with as a result, inventor's discovery is in three steps, the ratio of alkali lignin powder is gathered
The ratio of ethylene glycol, the revolving speed of spin duct, spin duct filament mouth are key factors at a distance from receipts filament plate.Different alkali lignins
The amount of powder and polyethylene glycol will affect the viscosity of spinning solution, and spinning solution is not easy to spray from spinning mouth when viscosity is big, on the contrary then difficult
At fiber；The revolving speed of spin duct determines the size for assigning the power that spinning solution is sprayed from spinning mouth, and revolving speed is faster, and centrifugal force is got over
Greatly, easier to be spun into fiber, but excessive revolving speed is also unfavorable for solvent volatilization, to be unfavorable for into fibre；Spinning visitor filament mouth with
The distance for receiving filament plate, which then influences volatilization time of solvent after spinning solution sprays, makes solvent preferably volatilize apart from larger, thus
Fiberizing is preferable.
By controlling the above key factor, the diameter minimum of resulting lignin-base fiber is up to 1 μm hereinafter, this is than tradition
Wet spinning, lignin-base fiber obtained by dry spinning and melt spinning small more of diameter, be also relatively shorter than by Static Spinning
The diameter for the lignin-base fiber that silk method obtains.Therefore, the beneficial effects of the present invention are by relatively simple method not
The lesser lignin-base fiber of diameter can only be prepared, this is not only to prepare lignin-base nano carbon fibre and nano active
Carbon fiber provides more excellent presoma, realizes the higher value application of lignin, and method of the invention is easy to operate,
It is less energy consumption, high-efficient, there is preferable prospects for commercial application.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of alkali lignin base fiber prepared by the embodiment of the present invention 1.
Fig. 2 is the scanning electron microscope (SEM) photograph of alkali lignin base fiber prepared by the embodiment of the present invention 2.
Fig. 3 is the scanning electron microscope (SEM) photograph of alkali lignin base fiber prepared by the embodiment of the present invention 3.
Fig. 4 is the scanning electron microscope (SEM) photograph of alkali lignin base fiber prepared by the embodiment of the present invention 4.
Fig. 5 is the scanning electron microscope (SEM) photograph of the alkali lignin base fiber of comparative example 1 of the present invention preparation.
Specific embodiment
Following embodiment further illustrates the contents of the present invention, but should not be construed as limiting the invention.Without departing substantially from
In the case where spirit of that invention and essence, to modifications or substitutions made by the method for the present invention, step or condition, the present invention is belonged to
Range.
Unless otherwise specified, the conventional means that technological means used in embodiment is well known to those skilled in the art,
In embodiment, each raw material of addition is commercially available conventional raw material unless otherwise indicated.
Embodiment 1
Pulping back liquor powder and suitable water are mixed, are after mixing evenly 10~15 μm qualitative with aperture
Filter paper filtering, removes the insoluble matter in black liquor.Take filtered filtrate that sulfuric acid is added several times, until the pH value of solution is adjusted to
2 or so, then with magnetic stirrer 30min, precipitating is then centrifugally separating to obtain using low speed centrifuge, gained is precipitated cold
It is lyophilized dry, finally grinds the alkali lignin powder that can be obtained by 100 mesh sieve for preparing spinning solution again.
Alkali lignin powder is dissolved in a certain amount of dimethyl formamide solution, adds polyethylene glycol (based on alkali
The 2% of lignin powder quality), and with dimethyl formamide solution by the mass fraction tune of alkali lignin powder and polyethylene glycol
It is whole to 50%, magnetic agitation 30min under the conditions of heating temperature is 60 DEG C obtains the spinning solution for preparing alkali lignin base fiber.
Then, by spinning solution be added centrifugal box-spinning machine spin duct in, adjustings spinning revolving speed be 8000 turns/min, spin duct filament mouth away from
The distance for receiving filament plate is 35cm, and it is 30 DEG C that environment temperature, which is arranged, relative humidity 60RH%.
The alkali lignin base fiber obtained using conditions above is as shown in Figure 1,40 fibers randomly selected by test
Diameter, and calculate average value, the diameter of gained alkali lignin base fiber is 2.5 μm.
Embodiment 2
Alkali lignin powder is prepared using the method in embodiment 1.Alkali lignin powder is dissolved in a certain amount of diformazan
In base formamide solution, polyethylene glycol (2% based on alkali lignin powder quality) is added, and use dimethyl formamide solution
The mass fraction of alkali lignin powder and polyethylene glycol is adjusted to 55%, magnetic agitation under the conditions of heating temperature is 70 DEG C
30min obtains the spinning solution for preparing alkali lignin base fiber.Then, spinning solution is added in the spin duct of centrifugal box-spinning machine, is adjusted
Section spinning revolving speed is 10000 turns/min, and spin duct filament mouth is 35cm away from the distance for receiving filament plate, and it is 32 that environment temperature, which is arranged,
DEG C, relative humidity 45RH%.
The alkali lignin base fiber obtained using conditions above is as shown in Fig. 2, 40 fibers randomly selected by test
Diameter, and calculate average value, the diameter of gained alkali lignin base fiber is 3.3 μm.
Embodiment 3
Alkali lignin powder is prepared using the method in embodiment 1.Alkali lignin powder is dissolved in a certain amount of diformazan
In base formamide solution, polyethylene glycol (1% based on alkali lignin powder quality) is added, and use dimethyl formamide solution
The mass fraction of alkali lignin powder and polyethylene glycol is adjusted to 55%, magnetic agitation under the conditions of heating temperature is 60 DEG C
30min obtains the spinning solution for preparing alkali lignin base fiber.Then, spinning solution is added in the spin duct of centrifugal box-spinning machine, is adjusted
Section spinning revolving speed is 12000 turns/min, and spin duct filament mouth is 50cm away from the distance for receiving filament plate, and it is 30 that environment temperature, which is arranged,
DEG C, relative humidity 55RH%.
The alkali lignin base fiber obtained using conditions above is as shown in figure 3,40 fibers randomly selected by test
Diameter, and calculate average value, the diameter of gained alkali lignin base fiber is 1.7 μm.
Embodiment 4
Alkali lignin powder is prepared using the method in embodiment 1.Alkali lignin powder is dissolved in a certain amount of diformazan
In base formamide solution, polyethylene glycol (1% based on alkali lignin powder quality) is added, and use dimethyl formamide solution
The mass fraction of alkali lignin powder and polyethylene glycol is adjusted to 60%, magnetic agitation under the conditions of heating temperature is 60 DEG C
30min obtains the spinning solution for preparing alkali lignin base fiber.Then, spinning solution is added in the spin duct of centrifugal box-spinning machine, is adjusted
Section spinning revolving speed is 14000 turns/min, and spin duct filament mouth is 50cm away from the distance for receiving filament plate, and it is 27 that environment temperature, which is arranged,
DEG C, relative humidity 70RH%.
The alkali lignin base fiber obtained using conditions above is as shown in figure 4,40 fibers randomly selected by test
Diameter, and calculate average value, the diameter of gained alkali lignin base fiber is 3.1 μm.
Comparative example 1
Alkali lignin powder is prepared using the method in embodiment 1.Alkali lignin powder is dissolved in a certain amount of diformazan
In base formamide solution, polyethylene glycol (1% based on alkali lignin powder quality) is added, and use dimethyl formamide solution
The mass fraction of alkali lignin powder and polyethylene glycol is adjusted to 35%, magnetic agitation under the conditions of heating temperature is 80 DEG C
30min obtains the spinning solution for preparing alkali lignin base fiber.Then, spinning solution is added in the spin duct of electrostatic spinning machine, is spun
Filament voltage is 25kV, and feed rate 0.5mL/h, spin duct filament mouth is 25cm away from the distance for receiving filament plate, and environment temperature is arranged
Degree is 25 DEG C, relative humidity 65RH%.
The alkali lignin base fiber obtained using conditions above is as shown in figure 5,40 fibers randomly selected by test
Diameter, and calculate average value, the diameter of gained alkali lignin base fiber is 5.1 μm.
It is compared to embodiment 1,2,3 and 4, using the diameter phase for the alkali lignin base fiber that electrospinning process is prepared
To the diameter for, showing preferably reduce alkali lignin base fiber using centrifugal spinning method more greatly；Also, the present invention uses
The mass fraction of spinning solution be higher than electrospinning process, the former spinning speed is also greater than the latter's.Therefore, this patent
Technical comparing is in existing common spinning process, not only less energy consumption, high-efficient, but also the diameter of the lignin-base fiber obtained obtains
To significant decrease, application value with higher.
The above is only that a specific embodiment of the invention is described, and is not intended to limit the scope of the present invention,
It should be pointed out that for those skilled in the art, without departing from the technical principles of the invention, existing
Several improvements and modifications can also be made on the basis of technology by having, these improvements and modifications should all should be regarded as right of the invention and want
In the protection scope for asking book to determine.
Claims (9)
1. a kind of preparation method of the alkali lignin base fiber with small diameter, which comprises the following steps:
(1) black liquor powder is mixed with water, is filtered after mixing evenly using filter paper, to remove larger particles insoluble matter in black liquor；
It takes filtrate that sulfuric acid is gradually added to be precipitated, precipitating is centrifugally separating to obtain using low speed centrifuge, gained pellet frozen is dry
After obtain alkali lignin powder；
(2) alkali lignin powder and polyethylene glycol are dissolved in dimethyl formamide solution in proportion in a heated condition, are obtained
To the spinning solution for preparing alkali lignin base fiber；
(3) spinning solution is added in spin duct, using centrifugal spinning method, adjusts spinning revolving speed, obtain alkali lignin base fiber.
2. preparation method according to claim 1, which is characterized in that in the step (1), gained alkali lignin powder is
Sulfuric acid precipitation is used from pulping back liquor, is centrifugally separating to obtain precipitating using low speed centrifuge, and pass through freeze-drying side
Method obtains powder, and it is levigate to more than 100 mesh to reuse mortar.
3. preparation method according to claim 1, which is characterized in that the polyethylene glycol of step (2) include molecular weight from
One of 100K-600K or a variety of.
4. preparation method according to claim 1, which is characterized in that the polyethylene glycol quality of step (2) is based on alkali wood
The quality of quality powder, ratio 0.5%-10%.
5. preparation method according to claim 1, which is characterized in that the alkali lignin powder and polyethylene glycol of step (2)
The mass fraction being dissolved in dimethyl formamide solution is 5%-70%.
6. preparation method as claimed in claim 5, which is characterized in that both alkali lignin powder and polyethylene glycol are in dimethyl
Heating temperature when dissolving in formamide solution is 25 DEG C -85 DEG C.
7. preparation method as described in claim 1, which is characterized in that the spin duct revolving speed of the centrifugal box-spinning machine of step (3) is
3000 turns/min-20000 turns/min, and spin duct filament mouth is 10cm-70cm away from the distance for receiving filament plate.
8. preparation method as claimed in claim 7, which is characterized in that the environment temperature of centrifugal spinning is controlled at 25 DEG C -35 DEG C,
Envionmental humidity is 20-80RH%.
9. the alkali lignin base fiber that any the method for claim 1-8 is prepared.
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| CN201810842740.8A CN109137139A (en) | 2018-07-27 | 2018-07-27 | A kind of preparation method of lignin-base fiber |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109111748A (en) * | 2018-07-04 | 2019-01-01 | 北京林业大学 | A kind of preparation method with good melting behaviour lignin |
| CN111672472A (en) * | 2020-06-23 | 2020-09-18 | 佛山(华南)新材料研究院 | Preparation method of degradable wood adsorption material |
| CN113529210A (en) * | 2021-06-28 | 2021-10-22 | 武汉纺织大学 | Lignin fiber for textile material and preparation method thereof |
| CN114601740A (en) * | 2021-12-16 | 2022-06-10 | 大连工业大学 | Preparation method of multifunctional natural lignin-based Pickering emulsion |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109111748A (en) * | 2018-07-04 | 2019-01-01 | 北京林业大学 | A kind of preparation method with good melting behaviour lignin |
| CN111672472A (en) * | 2020-06-23 | 2020-09-18 | 佛山(华南)新材料研究院 | Preparation method of degradable wood adsorption material |
| CN111672472B (en) * | 2020-06-23 | 2022-05-27 | 佛山(华南)新材料研究院 | Preparation method of degradable wood adsorption material |
| CN113529210A (en) * | 2021-06-28 | 2021-10-22 | 武汉纺织大学 | Lignin fiber for textile material and preparation method thereof |
| CN113529210B (en) * | 2021-06-28 | 2022-04-26 | 武汉纺织大学 | Lignin fiber for textile material and preparation method thereof |
| CN114601740A (en) * | 2021-12-16 | 2022-06-10 | 大连工业大学 | Preparation method of multifunctional natural lignin-based Pickering emulsion |
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