CN105386153A - Preparation method for ethyl cellulose micro-nanofibers - Google Patents
Preparation method for ethyl cellulose micro-nanofibers Download PDFInfo
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- CN105386153A CN105386153A CN201510823696.2A CN201510823696A CN105386153A CN 105386153 A CN105386153 A CN 105386153A CN 201510823696 A CN201510823696 A CN 201510823696A CN 105386153 A CN105386153 A CN 105386153A
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- ethyl cellulose
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- nano fiber
- cellulose micro
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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
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/18—Formation of filaments, threads, or the like by means of rotating spinnerets
-
- 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
- D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Artificial Filaments (AREA)
Abstract
The invention relates to the field of micro-nanofiber material preparation and aims at providing a preparation method for ethyl cellulose micro-nanofibers. The method comprises the following steps: mixing ethyl cellulose with polyoxyethylene and then dissolving in an ethanol water solution, and stirring under room temperature to obtain a spinning solution; performing centrifugal spinning on the spinning solution, and collecting by adopting a ring collecting method; immersing the ethyl cellulose micro-nanofibers into deionized water, soaking and washing under the room temperature, and after soaking, putting in a vacuum drying oven for drying to obtain the ethyl cellulose micro-nanofibers. The preparation method provided by the invention is simple, low in cost and high in efficiency, and has few process steps and a stable and efficient process; the used raw materials are low in cost and easy to get, and the application prospect and the application range in the fields of textile, filtration, biology, foodstuff, medical treatment and the like are broadened; a selected solvent is non-toxic, therefore not only is the environment protected but also the application reliability of the ethyl cellulose fibers in the fields of foodstuff, medical treatment, biology and the like is enhanced; an effective means is provided for batch preparation and scale production of the ethyl cellulose micro-nanofibers.
Description
Technical field
The invention belongs to micro nanometer fiber field of material preparation, be specifically related to a kind of preparation method of ethyl cellulose micro-and nano fiber.
Background technology
Cellulose is one of renewable resource the abundantest on the earth.According to statistics, in worldwide, the annual plant resources produced is up to 10,00,000,000,000 tons.Cellulose can be synthesized by water and carbon dioxide by photosynthesis, again can be degradable by microorganism in the Nature, and have good biocompatibility, therefore it is a kind of renewable resource and environment-friendly material.Cellulose is renewable due to it, the feature such as degradable and environmental friendliness, can be used for preparing the cellulose products of several functions, various cellulose derivative can also be prepared by derivative reaction, partly can replace petroleum resources, the disposable energy such as now oil face the problem such as shortage of resources, price rising make cellulose and its derivates as host material the potential scope of application widely, become the focus that countries in the world are competitively developed.At present, cellulose and its derivates has been widely used in weaving, plastics, papermaking, food, medicine, building, biology and the domain variability fast development such as military, and following cellulose and its derivates is by most possible one of important source material becoming chemical.
Ethyl cellulose is the cellulose derivative of suitability for industrialized production the earliest.The chemical stability of ethyl cellulose is very good, the various alkali of ability, diluted acid, salting liquid; Have excellent stability to light, Ultraviolet radiation can not make it variable color; Ethyl cellulose cellulose-based film and plastics have superior mechanical strength in very wide temperature range; Because it has unique and excellent performance, thus of many uses, main application has following aspect: be used for injection or extruded thin slice, film and coating layer material as plastic basis material; Hot-melt coating, strippable coatings, gel lacquer, paints, sprays paint; The sub-light film additive of polyvinyl chloride, binding agent, modifier, synthesized polymer material suspension polymerization dispersant; The fields such as medicine and food.
Cellulose derivative such as HEC, CMC, MC, HPMC, EC etc. have report by the technology of electrospun nanofibers more, but are just confined to laboratory research, and output is too low.
Centrifugal spinning technology is as a kind of important method preparing micro nanometer fiber, and in output, its single-nozzle can up to nearly thousand times compared with conventional electrostatic spinning; In raw material selection, centrifugal spinning is no longer by the restriction of material polarity.
Centrifugally spin in achievement in research existing, spinning material mainly adopts synthetic high polymer as PAN, PA6, PP, PBT, PMMA, PVP and PEO etc., its main cause is because synthetic high polymer strand is regular, unbranched or branching content is few, and relative molecular weight is high and narrow distribution range is suitable for spinning fibre, this also meets the General Requirements of fiber-forming polymer.But, natural polymer such as starch, cellulose etc. cause relative molecular weight distribution extensive because its source inherently there are differences, and branched-chain component is more or side base is huge on some main chain, this brings difficulty to the spinning of cellulose derivative, and namely simple solution of cellulose derivative is difficult to spinning.
In report known at present, as article " XiaohuiWu, LingeWang, etal..EffectofSolventonMorphologyofElectrospinningEthylC elluloseFibers [J] .JournalofAppliedPolymerScience, 2005, 97 (3): 1292-1297. " and " BilalAhmad, SimeonStoyanov, etal..Electrospinningofethylcellulosefibreswithglassands teelconfigurations [J] .FoodResearchInternational, 2013, 54 (2): 1761-1772. " in, the ethyl cellulose medicine choosing the higher narrow distribution range of relative molecular weight carries out laboratory research, but the drug price costliness after purifying only is suitable for laboratory research, production cannot be promoted, as in article " AudreyFrenot, MariaWaleniusHenriksson, etal..ElectrospinningofCellulose-BasedNanofibers [J] .JournalofAppliedPolymerScience, 2007, 103:1473 – 1482. ", adopt water miscible derivative to study, water-soluble solution met by the fiber produced like this, greatly limit its range of application, and for example " Um-i-Zahra, S., etal..Studyofsustainedreleasedrug-loadednanofibersofcell uloseacetateandethylcellulosepolymerblendspreparedbyelec trospinningandtheirin-vitrodrugreleaseprofiles [J] .JournalofPolymerResearch, 2014, 21 (12): 602-613. " etc. in some articles, the virose organic solvent dissolution ethyl cellulose of most use prepares nanofiber, poisonous organic solvent is adopted not only to there is potential safety hazard, also air or water pollution can be caused, be unfavorable for environmental protection, and these researchs are all adopt Static Spinning, productive rate is starkly lower than the spinning efficiency adopting centrifugal spinning technology.
At present, the report preparing ethyl cellulose micro-and nano fiber by centrifugal spinning technology not yet occurs.
Summary of the invention
The technical problem to be solved in the present invention is, overcomes deficiency of the prior art, provides a kind of method adopting nontoxic dual solvent system to prepare ethyl cellulose micro-and nano fiber fast.The method take ethyl cellulose as raw material, adds the polyethylene glycol oxide that can improve spinnability, and with second alcohol and water for solvent, by centrifugal spinning technology, adjustment solvent and relevant spinning condition parameter, successfully achieve the quick preparation of ethyl cellulose micro-and nano fiber.
For technical solution problem, solution of the present invention is:
A kind of preparation method of ethyl cellulose micro-and nano fiber is provided, comprises the following steps:
(1) centrifugal spinning prepares ethyl cellulose micro-and nano fiber
10 ~ 20: 1 by ethyl cellulose and polyethylene glycol oxide mixing in mass ratio, and being then dissolved in volume ratio is in the mixed solvent of second alcohol and water of 7: 3, stirred at ambient temperature 10 hours obtained spinning solutions; In spinning solution, the concentration of ethyl cellulose is 10 ~ 20% (w/v), and the concentration of polyethylene glycol oxide is 1% (w/v);
Be injected into by spinning solution in centrifugal spinning device, under the condition of rotating speed 3000 revs/min, receiving range 12 centimetres, carry out centrifugal spinning, adopt annular collection mode to collect ethyl cellulose micro-and nano fiber, the humidity that controls environment is 45 ± 5%;
(2) post-processing approach of ethyl cellulose micro-and nano fiber
Ethyl cellulose micro-and nano fiber is immersed in deionized water, soak 96 hours at normal temperatures; Took out every 24 hours in immersion process and repeat with deionized water to rinse, changing and soak deionized water used; After immersion completes, ethyl cellulose micro-and nano fiber is put into vacuum drying chamber, at 50 DEG C, drying 24 hours, obtains the ethyl cellulose micro-and nano fiber product eliminating polyethylene glycol oxide composition.
In the present invention, the viscosity of described ethyl cellulose is 18 ~ 330mPas, and the average molecular weight range of described polyethylene glycol oxide is 100,000 ~ 4,000,000.
In the present invention, the spinning device in described centrifugal spinning device adopts dispensing needle head as spinning head.
In the present invention, the diameter of the ethyl cellulose micro-and nano fiber prepared is 500nm ~ 10 μm.The diameter of ethyl cellulose micro-and nano fiber changes according to the needle diameter change used, and syringe needle more fibre diameter is less.
The invention has the beneficial effects as follows:
(1) the inventive method is simple to operate, and processing step is few, by centrifugal spinning technology; the fiber of micro/nano level can be obtained; process stabilization is efficient, is applicable to the large-scale production of ethyl cellulose, is also applicable to the spinning of variety classes cellulose derivative simultaneously.
(2) raw material used in the present invention are cheap and easy to get; the fiber of preparation can control between 500nm ~ 10 μm; its application prospect in fields such as weaving, filtration, biology, food and medical treatment and the scope of application are widened; slow down the pressure using synthetic material further, also can play a role in improving in environmental protection.
(3) selected solvent is nontoxic ethanol water mixed solvent, is both conducive to environmental protection, too increases the reliability of Ethyl Cellulose Fibers in field application such as food, medical treatment, biologies.
(4) this method is simple, cheap, efficient, and the batch for ethyl cellulose micro-and nano fiber prepares and large-scale production provides effective means.
Accompanying drawing explanation
Fig. 1 is SEM figure (amplifying 10000 times) of the Ethyl Cellulose Fibers that the embodiment of the present invention 1 obtains;
Fig. 2 is SEM figure (amplifying 1000 times) of the Ethyl Cellulose Fibers that the embodiment of the present invention 1 obtains;
Fig. 3 is SEM figure (amplifying 10000 times) of the Ethyl Cellulose Fibers that the embodiment of the present invention 2 obtains;
Fig. 4 is SEM figure (amplifying 1000 times) of the Ethyl Cellulose Fibers that the embodiment of the present invention 2 obtains;
Fig. 5 is SEM figure (amplifying 30000 times) of the Ethyl Cellulose Fibers that the embodiment of the present invention 3 obtains;
Fig. 6 is SEM figure (amplifying 5000 times) of the Ethyl Cellulose Fibers that the embodiment of the present invention 3 obtains.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described.
In the present invention, centrifugal spinning device used can adopt conventional centrifugal device for spinning, and spinning device wherein adopts dispensing needle head as spinning head.Because belonging to prior art, the present invention repeats no more.
Embodiment 1:
To be dissolved in the mixed solvent of 7mL ethanol and 3mL water (7:3) after 1g ethyl cellulose and 0.1g polyethylene glycol oxide (10:1) mixing, ethyl cellulose concentration is 10% (w/v), polyethylene glycol oxide concentration is 1% (w/v), stirred at ambient temperature 10 hours obtained spinning solutions.Ethyl cellulose viscosity parameter used is 330mPas, and polyethylene glycol oxide relative molecular weight is 4,000,000.
Being injected into by described spinning solution in centrifugal spinning device, is 3000 revs/min at rotating speed, and receiving range is carry out centrifugal spinning under the condition of 12 centimetres, select specification be the syringe needle of 25G as spinning head, annular collect, ambient humidity remains on 45 ± 5%.
Obtained fibrous material is immersed in deionized water, soak 96 hours at normal temperatures, took out above-mentioned fibrous material deionized water to repeat to rinse every 24 hours, and the immersion deionized water described in changing, finally fibrous material is put into vacuum drying chamber at 50 DEG C dry 24 hours, obtaining removing adding ingredient---the close absolutely fiber of cellulose content of polyethylene glycol oxide, diameter range is at 4 μm ~ 10 μm.
Embodiment 2:
To be dissolved in the mixed solvent of 7mL ethanol and 3mL water (7:3) after 1.5g ethyl cellulose and 0.1g polyethylene glycol oxide (15:1) mixing, ethyl cellulose concentration is 15% (w/v), polyethylene glycol oxide concentration is 1% (w/v), stirred at ambient temperature 10 hours obtained spinning solutions.Ethyl cellulose viscosity parameter used is 270mPas, and polyethylene glycol oxide relative molecular weight is 2,000,000.
Being injected into by described spinning solution in centrifugal spinning device, is 3000 revs/min at rotating speed, and receiving range is carry out centrifugal spinning under the condition of 12 centimetres, select specification be the syringe needle of 25G as spinning head, annular collect, ambient humidity remains on 45 ± 5%.
Obtained fibrous material is immersed in deionized water, soak 96 hours at normal temperatures, took out above-mentioned fibrous material deionized water to repeat to rinse every 24 hours, and the immersion deionized water described in changing, finally fibrous material is put into vacuum drying chamber at 50 DEG C dry 24 hours, obtaining removing adding ingredient---the close absolutely fiber of cellulose content of polyethylene glycol oxide, diameter range is at 3 μm ~ 8 μm.
Embodiment 3:
(20:1) after 1g ethyl cellulose and the mixing of 0.05g polyethylene glycol oxide is dissolved in the mixed solvent of 3.5mL ethanol and 1.5mL water (7:3), ethyl cellulose concentration is 20% (w/v), polyethylene glycol oxide concentration is 1% (w/v), stirred at ambient temperature 10 hours obtained spinning solutions, ethyl cellulose viscosity parameter used is 18mPas, polyethylene glycol oxide relative molecular weight is 1,000,000.
Being injected into by described spinning solution in centrifugal spinning device, is 3000 revs/min at rotating speed, and receiving range is carry out centrifugal spinning under the condition of 12 centimetres, select specification be the syringe needle of 25G as spinning head, annular collect, ambient humidity remains on 45 ± 5%.
Obtained fibrous material is immersed in deionized water, soak 96 hours at normal temperatures, took out above-mentioned fibrous material deionized water to repeat to rinse every 24 hours, and the immersion deionized water described in changing, finally fibrous material is put into vacuum drying chamber at 50 DEG C dry 24 hours, obtaining removing adding ingredient---the close absolutely fiber of cellulose content of polyethylene glycol oxide, diameter range is in 500nm ~ 3 μm.
It is noted that above example is only for illustration of the present invention, is convenient to those skilled in the art and understands technical conceive of the present invention and feature further, but do not limit the present invention in any form.It should be pointed out that those skilled in the art, without departing from the inventive concept of the premise, make various change or amendment to the present invention, these equivalent form of values belong to appended claims limited range of the present invention equally.
Claims (4)
1. a preparation method for ethyl cellulose micro-and nano fiber, is characterized in that, comprises the following steps:
(1) centrifugal spinning prepares ethyl cellulose micro-and nano fiber
10 ~ 20: 1 by ethyl cellulose and polyethylene glycol oxide mixing in mass ratio, and being then dissolved in volume ratio is in the mixed solvent of second alcohol and water of 7: 3, stirred at ambient temperature 10 hours obtained spinning solutions; In spinning solution, the concentration of ethyl cellulose is 10 ~ 20% (w/v), and the concentration of polyethylene glycol oxide is 1% (w/v);
Be injected into by spinning solution in centrifugal spinning device, under the condition of rotating speed 3000 revs/min, receiving range 12 centimetres, carry out centrifugal spinning, adopt annular collection mode to collect ethyl cellulose micro-and nano fiber, the humidity that controls environment is 45 ± 5%;
(2) post-processing approach of ethyl cellulose micro-and nano fiber
Ethyl cellulose micro-and nano fiber is immersed in deionized water, soak 96 hours at normal temperatures; Took out every 24 hours and repeatedly rinse with deionized water in immersion process, changing and soak deionized water used; After immersion completes, ethyl cellulose micro-and nano fiber is put into vacuum drying chamber, at 50 DEG C, drying 24 hours, obtains the ethyl cellulose micro-and nano fiber product eliminating polyethylene glycol oxide composition.
2. method according to claim 1, is characterized in that, the viscosity of described ethyl cellulose is 18 ~ 330mPas, and the average molecular weight range of described polyethylene glycol oxide is 1,000,000 ~ 4,000,000.
3. method according to claim 1, is characterized in that, the spinning device in described centrifugal spinning device adopts dispensing needle head as spinning head.
4. method according to claim 1, is characterized in that, the diameter of the ethyl cellulose micro-and nano fiber prepared is 500nm ~ 10 μm.
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| CN201510823696.2A CN105386153B (en) | 2015-11-24 | 2015-11-24 | The preparation method of ethyl cellulose micro-and nano fiber |
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| CN201510823696.2A CN105386153B (en) | 2015-11-24 | 2015-11-24 | The preparation method of ethyl cellulose micro-and nano fiber |
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| CN105386153B CN105386153B (en) | 2017-12-08 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108893792A (en) * | 2018-07-13 | 2018-11-27 | 深圳大学 | Bioactive fiber and preparation method thereof, application and preparation system |
| CN108939154A (en) * | 2018-07-16 | 2018-12-07 | 武汉纺织大学 | A kind of preparation method of collagen protein composite fiber bracket |
| CN110344127A (en) * | 2019-06-23 | 2019-10-18 | 浙江理工大学 | A kind of centrifugal spinning preparation method of porous Kynoar/polyethylene glycol oxide micro/nano-fibre |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN203782285U (en) * | 2014-04-28 | 2014-08-20 | 中山大学 | Micro-nanofiber centrifugal spinning device |
| CN104451912A (en) * | 2014-11-24 | 2015-03-25 | 浙江大学 | Preparing device and method for forming micro-nanofiber |
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- 2015-11-24 CN CN201510823696.2A patent/CN105386153B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN203782285U (en) * | 2014-04-28 | 2014-08-20 | 中山大学 | Micro-nanofiber centrifugal spinning device |
| CN104451912A (en) * | 2014-11-24 | 2015-03-25 | 浙江大学 | Preparing device and method for forming micro-nanofiber |
Non-Patent Citations (1)
| Title |
|---|
| 黄冬徽 等: "离心纺丝技术的发展现状", 《纺织导报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108893792A (en) * | 2018-07-13 | 2018-11-27 | 深圳大学 | Bioactive fiber and preparation method thereof, application and preparation system |
| CN108939154A (en) * | 2018-07-16 | 2018-12-07 | 武汉纺织大学 | A kind of preparation method of collagen protein composite fiber bracket |
| CN110344127A (en) * | 2019-06-23 | 2019-10-18 | 浙江理工大学 | A kind of centrifugal spinning preparation method of porous Kynoar/polyethylene glycol oxide micro/nano-fibre |
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| CN105386153B (en) | 2017-12-08 |
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