CN103937011B - A kind of cellulose dissolution liquid and preparation method and application - Google Patents
A kind of cellulose dissolution liquid and preparation method and application Download PDFInfo
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- CN103937011B CN103937011B CN201410146097.7A CN201410146097A CN103937011B CN 103937011 B CN103937011 B CN 103937011B CN 201410146097 A CN201410146097 A CN 201410146097A CN 103937011 B CN103937011 B CN 103937011B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention belongs to cellulose field, disclose a kind of cellulose dissolution liquid and preparation method and application.The preparation method of cellulose dissolution liquid of the present invention is: by certain mass percent mixed dissolution, organic solvent and ionic liquid are prepared mixed solvent；Again by cellulose through ultrasonic assistant dispersing and dissolving in described mixed solvent, obtain described cellulose dissolution liquid.In described cellulose dissolution liquid, cellulose mass fraction reaches 10%～25%.Described cellulose dissolution liquid can be applicable to electrical spinning method and prepares regenerated celulose fibre.Use the present invention can effectively solve cellulose indissoluble solution or dissolubility is low, spinning solution viscosity is high and the problem such as general fibre cellulose solution spinnability difference in usual vehicle, widen cellulose in chemical industry, the application of Material Field.
Description
Technical field
The invention belongs to cellulose field, be specifically related to a kind of cellulose dissolution liquid and preparation method and application.
Background technology
Cellulose is wide material sources, reproducible natural macromolecular material, be widely used in building materials,
The fields such as daily use chemicals, papermaking, food and medicine.But owing to native cellulose degree of crystallinity is high, intermolecular and molecule
Inside there is substantial amounts of hydrogen bond, noncrystalline domain is complicated so that it is be difficult to be dissolved in water and conventional organic solvent.Therefore,
Finding the effective dicyandiamide solution of cellulose, the method for research high-efficiency dissolution cellulose, to overcoming cellulose indissoluble
Solve, difficult melt and the defect such as the most plastic is significant.
Owing to conventional solvent dissolved efficiency is low, cost is high, heavy-polluted defect, twentieth century comes, and the world is each
State progressively turns to exploitation, and solubility property is good, easy to be recycled, the novel cellulose dissolution system of environmental protection.From
Sub-liquid, as the green solvent of a kind of alternative traditional chemical solvent, has begun working on its development both at home and abroad
And application, ion liquid solvent is respectively provided with good dissolubility to inorganic compound and organic compound, and it is also
There is high catalytic activity, stable chemical property, heat stability, highly polar, designability and repeatable time
Receive the advantages such as utilization.It is generally believed that the dissolving that cellulose is in ionic liquid is directly to dissolve, by destroying
With intramolecular hydrogen bond to reach the dissolving of cellulose between cellulosic molecule.Cellulose infiltrates in ionic liquid
First there occurs swollen, and then structure gradually occur loose, dissociate.Swatloski in 2002 et al. head
Secondary reporting can directly dissolve cellulose with ionic liquid, and lot of documents reports cellulose at ion afterwards
Dissolving in liquid and application.A kind of cellulose of United States Patent (USP) US20030157351 play-by-play is at ion
The method dissolved in liquid and process；The Chinese patent of Publication No. 1491974 and Publication No. 1818160 is public
Open the method utilizing several imidazolium ionic liquid to dissolve cellulose；Chinese patent ZL02823875.3(Shen
Please number 02823875.3) disclose employing ion liquid dissolving and the method for processing of cellulose.Above patent is all
Use ionic liquid as the solvent of cellulose.Although ionic liquid is the good solvent of cellulose, but cellulose and
The solution of ionic liquid composition generally also exists viscosity height and is unfavorable for the defect of processing.Ionic liquid is a kind of normal
The lower melted electrolyte of temperature, has good electric conductivity, and therefore, cellulose ion liquor possesses Electrospun
Advantage, but, if cellulose ion solution is applied to Electrospun, still need to solve solution viscosity
Problem.Army's equality research (Zhang Junping, the synthesis of rice husk cellulose derivant and applied research [D] thereof. Xi'an:
Northwest University 2002) mention in cellulose ionic liquid solution, add dimethyl sulfoxide (DMSO), energy
Promote that cellulose is swelling, stop strand to be assembled, reduce the effect of solution viscosity.But, add DMSO
Diluting effect can be played again while reducing viscosity, reduce the content of cellulose in solution, do not reach spinning
Concentration needed for solution.
Summary of the invention
In order to overcome the shortcoming of prior art with not enough, the primary and foremost purpose of the present invention is to provide a kind of cellulose
The preparation method of lysate, described preparation method uses organic solvent/ionic liquid mixed solvent to enter cellulose
Row dissolves, easy and simple to handle, and dissolved efficiency is high, and cellulose dissolution concentration is high, gained cellulose dissolution fluid viscosity
Low；
Another object of the present invention is to the cellulose dissolution liquid providing above-mentioned preparation method to obtain；
It is still another object of the present invention to provide the application of above-mentioned cellulose dissolution liquid.
The purpose of the present invention is achieved through the following technical solutions:
The preparation method of a kind of cellulose dissolution liquid, comprises the steps:
(1) add organic solvents in ionic liquid, stir, obtain mixed solvent；
Preferably, described organic solvent mass percent in described mixed solvent is 10%～20%；
Preferably, described organic solvent is DMF (DMF), N,N-dimethylacetamide
(DMAc) one or in dimethyl sulfoxide (DMSO)；It is furthermore preferred that described organic solvent is diformazan
Base sulfoxide；
Preferably, described ionic liquid is 1-ethyl-3-methylimidazole acetate ([Emim] Ac), 1-butyl-3
One in Methylimidazole. villaumite ([Bmim] Cl) or 1-pi-allyl-3-Methylimidazole. villaumite ([Amim] Cl)；
(2) cellulose is added in step (1) described mixed solvent, first carry out ultrasound wave dispersion, then enter
Row magnetic agitation makes described cellulose dissolution in described mixed solvent, obtains cellulose dissolution liquid；
Preferably, described cellulose is that alpha-cellulose powder, cotton pulp cellulose, cellulosic filter paper or needlebush are fine
One in dimension；It is furthermore preferred that described cellulose is alpha-cellulose powder；
Preferably, the degree of polymerization of described cellulose is 360～1460；
Preferably, described cellulose mass fraction in described cellulose dissolution liquid is 10%～25%；
Preferably, described cellulose, before adding mixed solvent, first activates；Concretely comprising the following steps of activation:
Cellulose is soaked in the sodium hydrate aqueous solution that mass fraction is 20% 1h, further takes out cellulose and use successively
Dehydrated alcohol and water washing, then by cellulose 60 DEG C of constant temperature in the vacuum drying oven that vacuum is-0.098KPa
It is dried 24h；
Preferably, described ultrasound wave scattered control parameter is: supersonic frequency is 16～24KHz, and power is
10～30W, the ultrasound works time is 3～5min, and working method is discontinuous operation, stops after the 1min that often works
1min；
Preferably, the control parameter of described magnetic agitation is: temperature is 90～100 DEG C, and stir speed (S.S.) is
200r/min, mixing time is 15～55min；
Preferably, described cellulose dissolution liquid carries out bubble removing process before preservation, concretely comprises the following steps: by institute
State cellulose dissolution liquid to be placed in 80 DEG C of vacuum drying ovens and carry out evacuation 2h；
A kind of cellulose dissolution liquid prepared according to said method.
The application in electrical spinning method prepares tModified Cellulose Fibers of the above-mentioned cellulose dissolution liquid；
Preferably, in above-mentioned application, the control condition of electrical spinning method is: spinning temperature is room temperature, spinning
Needle aperture is 0.6mm, and coagulation bath temperature is room temperature, and voltage is 40～50KV, electric spinning device shower nozzle with
Distance between collecting board is 25cm；
Preferably, the coagulator of described coagulating bath is ethanol or deionized water.
The principle of the present invention:
In preparation method of the present invention, between the anion of organic solvent energy reinforcing fiber element and ionic liquid
Interaction, destroy the interaction between anions and canons, the yin, yang in ionic liquid in ionic liquid
Ion again with the hydroxyl effect of cellulose, generate complex, destroy in cellulosic molecule with intermolecular hydrogen bond
System, thus accelerate the dissolving of cellulose；And organic solvent is as cosolvent, it is possible to substantially reduce ion
The viscosity of liquid.
The present invention has such advantages as relative to prior art and effect:
(1) preparation method of the present invention uses ionic liquid, there is higher ionic conductivity, can change
The electric conductivity of kind cellulose dissolution liquid, is advantageously applied to electrical spinning method and prepares cellulose fibre, for cellulose
Electrospun application provide wide research space.
(2) ionic liquid used in preparation method of the present invention has fixedness, is easily recycled and
The advantages such as utilization, and environmentally safe, it is possible to decrease production cost, economize on resources and the energy, is efficient
Green solvent.
(3) preparation method of the present invention can improve cellulose dissolubility in mix reagent, reduces fibre simultaneously
The viscosity of dimension element lysate, so that cellulose dissolution liquid is more conducive to carry out Electrospun prepares cellulose fibre,
Cost-effective can be easy to again spinning processing.
(4) preparation method of the present invention is used to dissolve cellulose, it is not necessary to carry out the technique such as yellow, maturation,
Being applicable to different composition, the dissolving of variety classes cellulose, raw material adjustable range is wide.
(5) cellulose dissolution liquid component of the present invention is uniform, and viscosity is low, it is easy to spinning.
Accompanying drawing explanation
Fig. 1 is raw material needle-leaved wood fibre in embodiment 1, product regenerated fiber silk and contrast product ion liquid
The FT-IR spectrogram of body regeneration needle-leaved wood fibre, in figure, a is the FT-IR curve of raw material needle-leaved wood fibre, b
For contrasting the FT-IR curve of product ion liquid regeneration needle-leaved wood fibre, c is that product needlebush of the present invention is fine
The FT-IR curve of dimension regenerated fiber silk.
Fig. 2 is raw material needle-leaved wood fibre in embodiment 1, product regenerated fiber silk and contrast product ion liquid
The XRD spectra of body regeneration needle-leaved wood fibre, in figure, a is the XRD spectral line of raw material needle-leaved wood fibre, and b is
The XRD spectral line of contrast product ion liquid regeneration needle-leaved wood fibre, c is product needle-leaved wood fibre of the present invention
The XRD spectral line of regenerated fiber silk.
Fig. 3 is cellulose polarizing microscope image of solute effect in mixed solvent, is respectively and dissolves
Solute effect when 0min, 2min, 10min and 30min.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but the embodiment party of the present invention
Formula is not limited to this.
Embodiment 1
A kind of cellulose dissolution liquid, preparation process is as follows:
(1) 1.0g N,N-dimethylformamide (DMF) and 4.00g1-ethyl-3-methylimidazole acetic acid are weighed
Salt ([Emim] Ac), under 60 DEG C of oil baths, magnetic agitation 10min makes its mix homogeneously, prepares
The mixed solvent of DMF/ [Emim] Ac.
(2) weigh in the balance and take the needle-leaved wood fibre of 5.0g, be 20% at 200mL, mass fraction under greenhouse
Sodium hydrate aqueous solution in process 1h, and with dehydrated alcohol and distilled water wash, then by cellulose in vacuum
Degree is 60 DEG C of freeze-day with constant temperature 24h in the vacuum drying oven of-0.098KPa, obtains the needle-leaved wood fibre of activation；?
In the mixed solvent of step (1) gained add 1.20g activation the pin wood fiber, rise high-temperature to 100 DEG C,
Ultrasound wave dispersion 3～5min, continues stirring 55min, obtains described cellulose dissolution liquid.
The viscosity of the most described cellulose dissolution liquid is 20cp, compared to pure [Emim] Ac to cellulose dissolution
System, viscosity degradation 51%.
Through electric spinning device, described cellulose dissolution liquid is carried out Electrospun, and coagulating bath is deionized water, temperature
Degree is 20 DEG C, and adjustment spinning voltage is 40kv, and spinning temperature is 25 DEG C, spinning needle aperture 0.6mm, spray
Head and collecting board spacing are 25cm.Start device for spinning and carry out Electrospun, coagulation tank is collected, obtains
The needle-leaved wood fibre regenerated fiber silk of a diameter of 1000nm, described regenerated fiber filament diameter is more uniform.
Use the Fourier transform infrared spectrometer (FT-IR Spectrometer) the raw material needle to the present embodiment
The wood fiber, end product regenerated fiber silk and according to prior art use pure [Emim] Ac ion liquid dissolving
Contrast product ion liquid regeneration needle-leaved wood fibre prepared by needle-leaved wood fibre is analyzed, gained FT-IR spectrogram
As it is shown in figure 1, wherein a is the FT-IR curve of raw material needle-leaved wood fibre in figure, b is contrast product ion liquid
The FT-IR curve of body regeneration needle-leaved wood fibre, c is the FT-IR curve of product regenerated fiber silk of the present invention.From
Fig. 1 can be seen that the regenerated fiber silk obtained by cellulose dissolution liquid electrospinning of the present invention, molecular structure with
Raw material needle-leaved wood fibre is compared and is held essentially constant, this explanation needle-leaved wood fibre mixing in the method for the invention
Bonding solvent is directly dissolve.
To raw material needle-leaved wood fibre, the end product regenerated fiber silk of the present embodiment and adopt according to prior art
The contrast product ion liquid regeneration needlebush prepared with pure [Emim] Ac ion liquid dissolving needle-leaved wood fibre is fine
Dimension carries out X-ray diffraction analysis, and gained XRD spectra is as in figure 2 it is shown, wherein a is raw material needlebush in figure
The XRD spectral line of fiber, b is the XRD spectral line of contrast product ion liquid regeneration needle-leaved wood fibre, and c is this
The XRD spectral line of invention product regenerated fiber silk.Knowable to the diffraction maximum shape of Fig. 2 and its position, needlebush
Dissolving in the most described mixed solvent of fiber and the structure in regenerative process there occurs change,
The crystal formation of needle-leaved wood fibre is transformed to fiber II type by fiber I type, and the destruction of original crystal formation makes needlebush
The degree of crystallinity of fiber reduces significantly.
Embodiment 2
A kind of cellulose dissolution liquid, preparation process is as follows:
(1) 0.50g DMAC N,N' dimethyl acetamide (DMAc) and 4.50g1-butyl-3-Methylimidazole. chlorine are weighed
Salt ([Bmim] Cl), under 60 DEG C of oil baths, magnetic agitation 10min makes its mix homogeneously, prepares
The mixed solvent of DMAc/ [Bmim] Cl.
(2) weigh in the balance and take the alpha-cellulose powder of 5.0g, be 20% at 200mL, mass fraction under greenhouse
Sodium hydrate aqueous solution in process 1h, and with dehydrated alcohol and distilled water wash, then by cellulose in vacuum
Degree is 60 DEG C of freeze-day with constant temperature 24h in the vacuum drying oven of-0.098KPa, obtains the alpha-cellulose powder of activation；?
In the mixed solvent of step (1) gained add 0.75g activation alpha-cellulose powder, rise high-temperature to 90 DEG C,
Ultrasound wave dispersion 3～5min, continues stirring 15min, obtains described cellulose dissolution liquid.
The viscosity of the most described cellulose dissolution liquid is 28cp, compared to pure [Bmim] Cl to cellulose dissolution
System, viscosity degradation 32%.
Through electric spinning device, described cellulose dissolution liquid is carried out Electrospun, and coagulating bath is deionized water, temperature
Degree is 20 DEG C, and adjustment spinning voltage is 50kv, and spinning temperature is 25 DEG C, spinning needle aperture 0.6mm, spray
Head and collecting board spacing are 25cm.Start device for spinning and carry out Electrospun, coagulation tank is collected, obtains
The alpha-cellulose powder regenerated fiber silk of a diameter of 700nm, described regenerated fiber filament diameter is more uniform.
Embodiment 3
A kind of cellulose dissolution liquid, preparation process is as follows:
(1) 1.00g dimethyl sulfoxide (DMSO) and 4.00g1-pi-allyl-3-Methylimidazole. villaumite are weighed
([Amim] Cl), under 60 DEG C of oil baths, magnetic agitation 10min makes its mix homogeneously, prepares
The mixed solvent of DMSO/ [Amim] Cl.
(2) weigh in the balance and take the cellulosic filter paper of 5.0g, be 20% at 200mL, mass fraction under greenhouse
Sodium hydrate aqueous solution in process 1h, and with dehydrated alcohol and distilled water wash, then by cellulose in vacuum
Degree is 60 DEG C of freeze-day with constant temperature 24h in the vacuum drying oven of-0.098KPa, obtains the cellulosic filter paper of activation；?
In mixed solvent described in step (1) add 1.1g activation cellulosic filter paper, rise high-temperature to 100 DEG C,
Ultrasound wave dispersion 3～5min, continues stirring 20min, obtains described cellulose dissolution liquid.
The viscosity of the most described cellulose dissolution liquid is 23cp, compared to pure [Amim] Cl to cellulose dissolution
System, viscosity degradation 44%.
Through electric spinning device, described cellulose dissolution liquid is carried out Electrospun, and coagulating bath is deionized water, temperature
Degree is 20 DEG C, and adjustment spinning voltage is 40kv, and spinning temperature is 25 DEG C, spinning needle aperture 0.6mm, spray
Head and collecting board spacing are 25cm.Start device for spinning and carry out Electrospun, coagulation tank is collected, obtains
The cellulosic filter paper regenerated fiber silk of a diameter of 850nm, described regenerated fiber filament diameter is more uniform.
Embodiment 4
A kind of cellulose dissolution liquid, preparation process is as follows:
(1) 0.50g dimethyl sulfoxide (DMSO) and 4.50g1-ethyl-3-methylimidazole acetate are weighed
([Emim] Ac), under 60 DEG C of oil baths, magnetic agitation 10min makes its mix homogeneously, prepares
The mixed solvent of DMSO/ [Emim] Ac.
(2) weigh in the balance and take the cotton pulp cellulose of 5.0g, be 20% at 200mL, mass fraction under greenhouse
Sodium hydrate aqueous solution in process 1h, and with dehydrated alcohol and distilled water wash, then by cellulose in vacuum
Degree is 60 DEG C of freeze-day with constant temperature 24h in the vacuum drying oven of-0.098KPa, obtains the cotton pulp cellulose of activation；?
In mixed solvent described in step (1) add 1.0g activation cotton pulp cellulose, rise high-temperature to 90 DEG C,
Ultrasound wave dispersion 3～5min, continues stirring 30min, obtains described cellulose dissolution liquid.
Under the polarizing microscope of band thermal station, observe cotton pulp cellulose in step (1) described DMSO/EMIMAc
Solute effect in mixed solvent, records the polarizing microscope image of its solute effect as it is shown on figure 3, divide
Wei not dissolve the solute effect of 0min, 2min, 10min and 30min.From observed result, cotton pulp is fine
Dimension element rate of dissolution in described mixed solvent is overall very fast.When 90 DEG C of temperature, cotton pulp cellulose is mixed
Abundant swollen in bonding solvent, the entangled state of molecule gradually releases, and cellulose molecular chain ruptures, and dissolves
Process starts progressively to accelerate.From the figure 3, it may be seen that cotton pulp cellulose begins to dissolve during 2min, 10min
Rear cotton pulp cellulose major part is dissolved, along with the rate of dissolution carrying out cellulose dissolved has declined,
This is because the reason that now cellulose solution concentration is gradually increased, arrive 30min cellulose and be completely dissolved,
The most substantially obvious cellosilk is not observed in the visual field.
The cellulose dissolution liquid obtaining the present embodiment carries out viscosity test, the viscosity of described cellulose dissolution liquid
For 25cp, compared to pure [Emim] Ac to cellulose dissolution system, viscosity degradation 40%.
Through electric spinning device, the cellulose spin dope dissolved is carried out Electrospun, and coagulating bath is deionization
Water, temperature is 20 DEG C, and adjustment spinning voltage is 50kv, and spinning temperature is 25 DEG C, spinning needle aperture 0.6mm,
Shower nozzle and collecting board spacing are 25cm.Start device for spinning and carry out Electrospun, coagulation tank is collected,
To the cotton pulp tModified Cellulose Fibers silk of a diameter of 600nm, described regenerated cellulose diameter is more uniform.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by above-mentioned enforcement
The restriction of example, the change made, modifies, replaces under other any spirit without departing from the present invention and principle
In generation, combine, simplify, all should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (7)
1. the preparation method of a cellulose dissolution liquid, it is characterised in that comprise the steps:
(1) add organic solvents in ionic liquid, stir, obtain mixed solvent；
Described organic solvent is in N,N-dimethylformamide, DMAC N,N' dimethyl acetamide or dimethyl sulfoxide
One, described ionic liquid is 1-ethyl-3-methylimidazole acetate, 1-butyl-3 Methylimidazole. villaumite or 1-
One in pi-allyl-3-Methylimidazole. villaumite；
(2) cellulose is added in step (1) described mixed solvent, first carry out ultrasound wave dispersion, then enter
Row magnetic agitation makes described cellulose dissolution in described mixed solvent, obtains cellulose dissolution liquid；Step (1)
Described in organic solvent mass percent in described mixed solvent be 10%～20%；Institute in step (2)
Stating cellulose is the one in alpha-cellulose powder, cotton pulp cellulose, cellulosic filter paper or needle-leaved wood fibre；Institute
The degree of polymerization stating cellulose is 360～1460；Described cellulose mass fraction in described cellulose dissolution liquid
It is 10%～25%；Ultrasound wave scattered control parameter described in step (2) is: supersonic frequency is 16～24KHz,
Power is 10～30W, and the ultrasound works time is 3～5min, and working method is discontinuous operation, and often work 1min
Rear stopping 1min；Described in step (2), the control parameter of magnetic agitation is: temperature is 90～100 DEG C, stirs
The time of mixing is 15～55min；
Described cellulose, before adding mixed solvent, first activates, concretely comprising the following steps of activation: by fiber
Element soaks 1h in the sodium hydrate aqueous solution that mass fraction is 20%, further takes out cellulose and uses anhydrous second successively
Alcohol and water washs, then by cellulose 60 DEG C of freeze-day with constant temperature in the vacuum drying oven that vacuum is-0.098KPa
24h。
The preparation method of cellulose dissolution liquid the most according to claim 1, it is characterised in that: step
(1) organic solvent described in is dimethyl sulfoxide；Described in step (2), cellulose is alpha-cellulose powder.
The preparation method of cellulose dissolution liquid the most according to claim 1, it is characterised in that:
Described in step (2), the control parameter of magnetic agitation is: stir speed (S.S.) is 200r/min.
The preparation method of cellulose dissolution liquid the most according to claim 1, it is characterised in that described fibre
Dimension element lysate carries out bubble removing process before preservation, concretely comprises the following steps: be placed in by described cellulose dissolution liquid
80 DEG C of vacuum drying ovens carry out evacuation 2h.
5. the cellulose dissolution liquid obtained according to the preparation method described in any one of Claims 1-4.
Cellulose dissolution liquid the most according to claim 5 prepares tModified Cellulose Fibers at electrical spinning method
In application.
Application the most according to claim 6, it is characterised in that: the control condition of electrical spinning method is:
Spinning temperature is room temperature, and spinning needle aperture is 0.6mm, and coagulation bath temperature is room temperature, and voltage is 40～50KV,
Distance between electric spinning device shower nozzle and collecting board is 25cm；The coagulator of described coagulating bath be ethanol or go from
Sub-water.
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104151622B (en) * | 2014-08-08 | 2016-09-07 | 华中科技大学 | A kind of biodegradable cellulose intermingling material and preparation method thereof |
| CN105506779B (en) * | 2016-01-13 | 2017-10-17 | 江苏科技大学 | Mulberry bamboo composite of graft modification mulberry fiber and bamboo fibre and preparation method thereof in ionic liquid |
| CN106283239A (en) * | 2016-08-09 | 2017-01-04 | 东华大学 | A kind of concentration cellulose element spinning liquid spinning technique |
| CN106283245A (en) * | 2016-08-09 | 2017-01-04 | 东华大学 | A kind of spinning technique of small molecule liquid crystal modified cellulose fibre |
| CN107630257B (en) * | 2017-09-18 | 2019-07-30 | 浙江纺织服装职业技术学院 | A kind of method of cellulose electrostatic spinning |
| CN107699966B (en) * | 2017-09-18 | 2019-07-30 | 浙江纺织服装职业技术学院 | A kind of method of cellulose electrostatic spinning |
| CN108187408A (en) * | 2017-12-27 | 2018-06-22 | 中国科学院化学研究所 | A kind of room temperature cleaning method of filter element |
| CN110172746B (en) * | 2019-05-30 | 2020-07-28 | 当阳市鸿阳新材料科技有限公司 | Method for preparing lyocell fibers by dissolving cellulose in solvent |
| CN110656380A (en) * | 2019-09-10 | 2020-01-07 | 北京理工大学 | Method for preparing different-form cellulose materials by electrostatic spinning based on ionic liquid |
| CN111116951B (en) * | 2020-01-06 | 2022-08-09 | 广西大学 | Method for preparing regenerated fiber film by using waste corrugated board |
| CN112029119B (en) * | 2020-08-03 | 2022-10-25 | 福建农林大学 | Method for efficiently and quickly dissolving cellulose |
| CN116102746B (en) * | 2023-02-20 | 2024-04-12 | 四川大学 | Method for dissolving cellulose based on proton type ionic liquid |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1491974A (en) * | 2002-10-22 | 2004-04-28 | 中国科学院化学研究所 | Cellulose solution and its preparing method |
| CN101240085A (en) * | 2007-02-08 | 2008-08-13 | 中国纺织科学研究院 | Cellulose solution and preparation thereof thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1491974A (en) * | 2002-10-22 | 2004-04-28 | 中国科学院化学研究所 | Cellulose solution and its preparing method |
| CN101240085A (en) * | 2007-02-08 | 2008-08-13 | 中国纺织科学研究院 | Cellulose solution and preparation thereof thereof |
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