CN105780184A - Method for preparing fiber from carboxymethyl cellulose (CMC) by electrostatic spinning - Google Patents
Method for preparing fiber from carboxymethyl cellulose (CMC) by electrostatic spinning Download PDFInfo
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- CN105780184A CN105780184A CN201610342421.1A CN201610342421A CN105780184A CN 105780184 A CN105780184 A CN 105780184A CN 201610342421 A CN201610342421 A CN 201610342421A CN 105780184 A CN105780184 A CN 105780184A
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- electrostatic spinning
- cellulose
- carboxymethyl cellulose
- cmc
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
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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
- 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
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
Abstract
The invention discloses a method for preparing fiber from carboxymethyl cellulose (CMC) by electrostatic spinning and relates to the technical field of electrostatic spinning. The method disclosed by the invention has the advantages that a polyvinyl alcohol (PVA) solution and acidified carboxymethyl cellulose suspension are added into an aqueous system of CMC, the spinnability of CMC is effectively improved; and the diameter of the obtained nanofiber is about 300nm, and the nanofiber is bright and clean in surface, good in continuity, uniform in fineness and narrow in fineness dispersion.
Description
Technical field
The present invention relates to electrostatic spinning technique field, particularly to the technical field of Biodegradable nano material and electrostatic spinning.
Background technology
Method of electrostatic spinning is the technology of a kind of high-efficiency production of nano fiber, the high polymer of formation non-Newtonian fluid or molten mass are under the effect breaking through high-pressure electrostatic power, forming nanofiber, the non-Newtonian fluid only with instability just can carry out electrostatic spinning, and this is one of the basic feature of the method.Not only multiple synthesis can be become single nanofiber with natural polymer electrospinning, it is also possible to obtain composite nano-fiber material, for instance the application of the technology such as coaxial spinning, three axle spinning, multilamellar intersection spinning, promote the fast development of this technology.
Good characteristic due to nano-fiber material performance, at film filter, tissue engineering bracket, biological engineering, clinical medicine, super dependent sensor, the aspect such as lithium battery material and ultracapacitor has huge researching value, but, the common polymer kind that can carry out electrostatic spinning at present is also relatively fewer, it is concentrated mainly on polyvinyl alcohol (PVA), polyacrylonitrile (PAN), polyvinylpyrrolidone (PVP) etc., and the electrostatic spinning of polysaccharose substance and natural polymer is studied the difficult point being always up this field, extremely limit the further development of electrostatic spinning research.
Cellulose and derivant are one of resources having scale prospect most, have the researching value that other materials is incomparable, and such material has been subject to the extensive concern of scholar in electrostatic spinning research.It is referred to as the advantage that the carboxymethyl cellulose (CMC) of " industry monosodium glutamate " has other materials incomparable, its cost is low, easily water-soluble, environmental friendliness, technique are simple, are widely used in the fields such as oil, coating, food, membrane material, pottery, medicine, battery, aviation and wide.But due to its own structure and performance, its suitable Electrospun approach rarely has report always.
Summary of the invention
Goal of the invention: for the deficiencies in the prior art, the present invention proposes the method that carboxymethyl cellulose (CMC) can be spun into fiber by one.
The present invention comprises the following steps:
1) microcrystalline Cellulose and concentrated sulphuric acid being mixed, stirring reaction under 45 DEG C of conditions, reaction adds distilled water after terminating, and obtains turbid liquid；
2) with turbid liquid described in distilled water centrifuge washing, proceed in bag filter, put in deionized water and dialyse, when the pH value of deionized water reaches neutrality, obtain Cellulose nanocrystal suspension；
3) carboxymethyl cellulose (CMC) and polyvinyl alcohol (PVA) are dissolved in deionized water, obtain carboxymethyl cellulose (CMC) and the mixed solution of polyvinyl alcohol (PVA), again mixed solution is mixed with Cellulose nanocrystal suspension, stand after magnetic agitation, obtain removing the electrostatic spinning solution of bubble；
4) electrostatic spinning: by described electrostatic spinning solution through Static Spinning, obtains fiber.
In step 1) of the present invention, the concentration of concentrated sulphuric acid is the optium concentration obtained through overtesting, and 45 DEG C of acidolysis can ensure that microcrystalline Cellulose obtains sufficient acidolysis, and as used higher temperature, cellulose can interior carbonization at short notice.And low temperature can consume the longer response time, and Product size is it cannot be guaranteed that homogeneous.
The present invention is by addition polyvinyl alcohol (PVA) solution in carboxymethyl cellulose (CMC) aqueous phase system and the suspension liquid of carboxyl methyl cellulose after acidolysis, effectively improve the spinnability of carboxymethyl cellulose (CMC), the nanofiber diameter thus obtained is about 300nm, show bright and clean, seriality is good, even thickness, fineness degree dispersion is narrower.
Further, in step 1) of the present invention, the degree of polymerization of microcrystalline Cellulose is 210～240, diameter 10～20 μm, length 100～200 μm.
It addition, in described step 1), the mixed volume ratio of concentrated sulphuric acid and distilled water is 1: 1, the mixing ratio of microcrystalline Cellulose and concentrated sulphuric acid is 1g: 8～15mL.If the too low meeting of concentrated sulphuric acid concentration causes the situation that acidolysis is insufficient, excessive concentration is easily caused cellulose carbonization.
In described step 1), mixing speed is 200～600r/min.If rotating speed is too low, will be unable to dispersion cellulose and make its abundant acidolysis, if rotating speed is too high, it may appear that bad phenomenon such as pole-climbings.
Described step 2) in every time centrifugal 10min, centrifuge speed 9000rmp/min.Cellulose is scattered in water with solvent swelling state, if rotating speed is too low, it is impossible to be centrifuged by cellulose insufficient for acidolysis, and rotating speed reaches 9000 just passable, and rotating speed is too high be there is no need.
In the electrostatic spinning solution of described removal bubble, the quality accounting of carboxymethyl cellulose (CMC) is 1.0%, and the quality accounting of polyvinyl alcohol (PVA) is 2.0%, and the quality accounting of nanocrystalline cellulose (NCC) is 0.7%.Test result indicate that, the addition of simple nanocrystalline cellulose (NCC) suspension can not improve the spinnability of CMC well, fiber surface pattern is not bright and clean, and thickness is uneven, after adding appropriate PVA solution, effectively widen the spinning window of CMC, and gained fibre diameter is about 300nm, any surface finish, seriality is good, even thickness, disperses narrower.
In described step 4), during Static Spinning, needle point and the distance received between device of electrostatic spinning apparatus are 15cm, and solution flow rate is 0.85ml/h, and voltage is 18kV, and the fiber morphology obtained under this condition is ideal.
Accompanying drawing explanation
Fig. 1 is the optical microscope photograph that embodiment 1 prepares gained fiber.
Fig. 2 is the optical microscope photograph that comparative example 1 prepares gained fiber.
Fig. 3 is the optical microscope photograph that comparative example 2 prepares gained fiber.
Fig. 4 is the stereoscan photograph that embodiment 1 prepares gained fiber.
Fig. 5 is the stereoscan photograph that comparative example 1 prepares gained fiber.
Fig. 6 is the stereoscan photograph that comparative example 2 prepares gained fiber.
Fig. 7 is the diameter distribution profile that embodiment 1 prepares gained fiber.
Fig. 8 is the diameter distribution profile that comparative example 2 prepares gained fiber.
Detailed description of the invention
Other advantages of the present invention and effect by detailed description below continuing on.
One, embodiment 1:
1,5g microcrystalline Cellulose and the concentrated sulphuric acid that 50mL concentration is 64wt% being mixed, under 45 DEG C of conditions, be that 200～600r/min is stirred reaction through speed, reaction adds appropriate distilled water after terminating, and obtains turbid liquid.
The microcrystalline Cellulose degree of polymerization adopted is 210～240, diameter 10～20 μm, length 100～200 μm.
2, with the above-mentioned turbid liquid of distilled water centrifuge washing 3 to 5 times, centrifugal 10min every time, centrifuge speed 9000rmp/min, it is then combined with the liquid phase that centrifuging and taking obtains and is placed in bag filter, put in deionized water and dialyse, the pH value of periodic detection deionized water, when the pH value of deionized water reaches neutrality, obtains the Cellulose nanocrystal suspension in bag filter.
Add appropriate distilled water after recording suspension quality concentration, obtain the Cellulose nanocrystal suspension that mass concentration is 1.4wt%.
3,0.4g carboxymethyl cellulose (CMC) and 0.8g polyvinyl alcohol (PVA) are dissolved in 18.8g deionized water, obtain 20g carboxymethyl cellulose (CMC) and the mixed solution of polyvinyl alcohol (PVA).
Again above-mentioned mixed solution is mixed with the Cellulose nanocrystal suspension that 20g concentration is 1.4wt%, stand after magnetic agitation, obtain removing the electrostatic spinning solution of bubble.
Through analysis point, in the electrostatic spinning solution removing bubble, the quality accounting of carboxymethyl cellulose (CMC) is 1.0%, and the quality accounting of polyvinyl alcohol (PVA) is 2.0%, and the quality accounting of nanocrystalline cellulose (NCC) is 0.7%.
4, by described electrostatic spinning solution through Static Spinning, needle point and the distance received between device of electrostatic spinning apparatus are 15cm, and solution flow rate is 0.85ml/h, and voltage is 18kV, obtains fiber.
Two, comparative example 1:
1,0.2g carboxymethyl cellulose (CMC) is dissolved in 19.8g deionized water, obtains 20g carboxymethyl cellulose (CMC) solution.
Through analysis point, in the electrostatic spinning solution removing bubble, the quality accounting of carboxymethyl cellulose (CMC) is 1.0%.
2, by carboxymethyl cellulose (CMC) solution through Static Spinning, needle point and the distance received between device of electrostatic spinning apparatus are 15cm, and solution flow rate is 0.85ml/h, and voltage is 18kV, obtains fiber.
Three, comparative example 2:
1,5g microcrystalline Cellulose and the sulphuric acid that 50mL concentration is 64wt% being mixed, stirring reaction under 45 DEG C of conditions, reaction adds appropriate distilled water after terminating, and obtains turbid liquid.
The microcrystalline Cellulose degree of polymerization adopted is 210～240, diameter 10～20 μm, length 100～200 μm.
2, with the above-mentioned turbid liquid of distilled water centrifuge washing 3 to 5 times, centrifugal 10min every time, centrifuge speed 9000rmp/min, it is then combined with the liquid phase that centrifuging and taking obtains and is placed in bag filter, put in deionized water and dialyse, the pH value of periodic detection deionized water, when the pH value of deionized water reaches neutrality, obtains the Cellulose nanocrystal suspension in bag filter.
Add appropriate distilled water after recording suspension quality concentration, obtain the Cellulose nanocrystal suspension that mass concentration is 1.4wt%.
3,0.4g carboxymethyl cellulose (CMC) is dissolved in 19.6g deionized water, obtains 20g carboxymethyl cellulose (CMC) solution.
Again above-mentioned carboxymethyl cellulose (CMC) solution is mixed with the Cellulose nanocrystal suspension that 20g concentration is 1.4wt%, stand after magnetic agitation, obtain removing the electrostatic spinning solution of bubble.
Through analysis point, in the electrostatic spinning solution removing bubble, the quality accounting of carboxymethyl cellulose (CMC) is 1.0%, and the quality accounting of nanocrystalline cellulose (NCC) is 0.7%.
4, by described electrostatic spinning solution through Static Spinning, needle point and the distance received between device of electrostatic spinning apparatus are 15cm, and solution flow rate is 0.85ml/h, and voltage is 18kV, obtains fiber.
Three, result is analyzed:
Fig. 1,2,3 respectively embodiment 1, comparative example 1, comparative example 2 prepare the optical microscope photograph of gained fiber.It can be seen that the fiber seriality that embodiment 1 prepares is good, diameter is more uniform, and comparative example 1 is containing only CMC solution, formation mostly be drop, it is difficult to form continuous fiber, comparative example 2 add appropriate NCC, it is possible to form continuous fiber, but pattern is not as good as embodiment 1.
Fig. 4,5,6 are the stereoscan photograph that embodiment 1, comparative example 1, comparative example 2 prepare gained fiber respectively.Can be seen that embodiment 1 is prepared gained fiber and shown bright and clean, seriality is good, even thickness, disperses narrower, and comparative example 1 mostly is drop, and comparative example 2 can prepare continuous fiber, but fiber thickness differs, and diameter Distribution is wider.
Fig. 7,8 respectively embodiment 1, comparative example 2 prepare the diameter distribution profile of gained fiber, it can be seen that although both average diameters are more or less the same, but the distribution that embodiment 1 prepares gained fiber is significantly narrower than comparative example 2.Visible, method proposed by the invention can effectively improve the electrospinning of CMC, and the optimum formula that described concentration is CMC spinning.
Claims (7)
1. carboxymethyl cellulose is carried out the method that electrostatic spinning makes fiber by one kind, it is characterised in that comprise the following steps:
1) microcrystalline Cellulose and concentrated sulphuric acid being mixed, stirring reaction under 45 DEG C of conditions, reaction adds distilled water after terminating, and obtains turbid liquid；
2) with turbid liquid described in distilled water centrifuge washing, proceed in bag filter, put in deionized water and dialyse, when the pH value of deionized water reaches neutrality, obtain Cellulose nanocrystal suspension；
3) carboxymethyl cellulose and polyvinyl alcohol are dissolved in deionized water, obtain the mixed solution of carboxymethyl cellulose and polyvinyl alcohol, then mixed solution is mixed with Cellulose nanocrystal suspension, stand after magnetic agitation, obtain removing the electrostatic spinning solution of bubble；
4) by described electrostatic spinning solution through Static Spinning, fiber is obtained.
2. preparation method according to claim 1, it is characterised in that in described step 1), the degree of polymerization of microcrystalline Cellulose is 210～240, diameter 10～20 μm, length 100～200 μm.
3. preparation method according to claim 1, it is characterised in that in described step 1), the mixed volume ratio of concentrated sulphuric acid and distilled water is 1: 1, the mixing ratio of microcrystalline Cellulose and concentrated sulphuric acid is 1g: 8～15mL.
4. preparation method according to claim 1, it is characterised in that in described step 1), mixing speed is 200～600r/min.
5. preparation method according to claim 1, it is characterised in that described step 2) in centrifuge speed 9000rmp/min.
6. preparation method according to claim 1, it is characterised in that in the electrostatic spinning solution of described removal bubble, the quality accounting of carboxymethyl cellulose is 1.0%, and the quality accounting of polyvinyl alcohol is 2.0%, and the quality accounting of nanocrystalline cellulose is 0.7%.
7. preparation method according to claim 1, it is characterised in that in described step 4), during Static Spinning, needle point and the distance received between device of electrostatic spinning apparatus are 15cm, and solution flow rate is 0.85ml/h, and voltage is 18kV.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106929929A (en) * | 2017-03-21 | 2017-07-07 | 昆明理工大学 | A kind of preparation method of the cellulose spin dope for electrostatic spinning |
| CN107201563A (en) * | 2017-06-09 | 2017-09-26 | 上海交通大学 | A kind of preparation method of the colored fiber based on Cellulose nanocrystal |
| US20180114967A1 (en) * | 2016-10-24 | 2018-04-26 | Samsung Electronics Co., Ltd | Separator, electrochemical cell including separator, method of preparing separator, and non-woven fabric |
| CN108286082A (en) * | 2018-03-08 | 2018-07-17 | 唐卫兵 | A kind of preparation method of efficiently moisture-proof multilayer alkyd resin nano-cellulose spinning solution |
| CN109674721A (en) * | 2019-01-31 | 2019-04-26 | 杭州恒邦实业有限公司 | A kind of preparation method of carboxymethyl cellulose fiber facial mask |
| CN113355315A (en) * | 2021-05-31 | 2021-09-07 | 扬州大学 | Preparation method of pullulan-animal esterase composite nanofiber |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20180114967A1 (en) * | 2016-10-24 | 2018-04-26 | Samsung Electronics Co., Ltd | Separator, electrochemical cell including separator, method of preparing separator, and non-woven fabric |
| CN106929929A (en) * | 2017-03-21 | 2017-07-07 | 昆明理工大学 | A kind of preparation method of the cellulose spin dope for electrostatic spinning |
| CN106929929B (en) * | 2017-03-21 | 2019-06-07 | 昆明理工大学 | A kind of preparation method of the cellulose spin dope for electrostatic spinning |
| CN107201563A (en) * | 2017-06-09 | 2017-09-26 | 上海交通大学 | A kind of preparation method of the colored fiber based on Cellulose nanocrystal |
| CN107201563B (en) * | 2017-06-09 | 2019-07-12 | 上海交通大学 | A kind of preparation method of the colored fiber based on Cellulose nanocrystal |
| CN108286082A (en) * | 2018-03-08 | 2018-07-17 | 唐卫兵 | A kind of preparation method of efficiently moisture-proof multilayer alkyd resin nano-cellulose spinning solution |
| CN109674721A (en) * | 2019-01-31 | 2019-04-26 | 杭州恒邦实业有限公司 | A kind of preparation method of carboxymethyl cellulose fiber facial mask |
| CN113355315A (en) * | 2021-05-31 | 2021-09-07 | 扬州大学 | Preparation method of pullulan-animal esterase composite nanofiber |
| CN113355315B (en) * | 2021-05-31 | 2023-11-03 | 扬州大学 | Preparation method of pullulan-animal esterase composite nanofiber |
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