CN104032400B - Biology enzyme/lignocellulose composite fibre and preparation method thereof - Google Patents
Biology enzyme/lignocellulose composite fibre and preparation method thereof Download PDFInfo
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- CN104032400B CN104032400B CN201410275053.4A CN201410275053A CN104032400B CN 104032400 B CN104032400 B CN 104032400B CN 201410275053 A CN201410275053 A CN 201410275053A CN 104032400 B CN104032400 B CN 104032400B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000009987 spinning Methods 0.000 claims abstract description 61
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Abstract
The present invention relates to a kind of biology enzyme/lignocellulose composite fibre and preparation method thereof, comprise step: lignocellulose fragment is dissolved in N-ethylpyridine villaumite ([bmim] Cl)/1-ethyl-3-methylimidazole borate ([bmim] [BF by (1)
4]) in mixed room temperature ionic liquid, form homogeneous phase solution; (2) papain powder is dissolved in the solution that step (1) prepares according to certain mass percent, obtain homogeneous phase blend spinning stoste; (3) spinning solution forms dynamic analysis of spinning after being extruded by spinning head after deaeration, filtration, metering, enter coagulating bath solidification forming, carry out wet spinning and electrostatic spinning after adopting even spinning solution blended, the method have environmental protection, cost is low, spinning speed is fast, production efficiency advantages of higher; The composite fibre prepared is compared with traditional textile fiber material, and have the advantages such as comfortable, output is large, textile process becomes fabric, and finally can make the textiles carrying biology enzyme energy beauty treatment skin, as underwear, brassiere, socks, bady's diaper etc.
Description
technical field:
The present invention relates to a kind of cellulose composite fiber and preparation method thereof, particularly relate to a kind of biology enzyme/lignocellulose composite fibre and preparation method thereof.
background technology:
Synthetic fiber experienced by semicentennial fast development, and the simultaneous petroleum resources reality increased with environmental protection pressure in short supply, the comprehensive utilization of natural resources more and more comes into one's own.
Cellulose and biology enzyme are all important natural materials, and wherein cellulose is formed by the photosynthesis of plant, and people are referred to as " green material ".This kind of reproducible living resources can be described as inexhaustible, it is applicable to various practical application, slow down the environmental pollution that asking for and thus cause of the mankind to mineral resources widely.Especially become in the large atmosphere of mankind's focus in current environmental pollution, cellulose substrate material causes the concern of people more, in national economy and daily life, have irreplaceable critical role.
Native cellulose fibre mainly comes from string, and people utilize cellulose fibre to have the history of several thousand, as fibers such as cotton, fiber crops, timber, bamboos.Cellulose substrate material, also claims wood materials.It comprises timber (wood-base fibre and particle panel material), cotton (artificial cotton), crudefiber crop and paper products etc.The raw material of material is taken from the plant that nature extensively exists.Timber is taken from the part of becoming a useful person of arbor.It is formed primarily of cellulose, hemicellulose and lignin, and cellulose and hemicellulose are generically and collectively referred to as holocellulose.Lignin, cellulose and hemicellulose are the main components forming plant skeleton.He Yanfeng etc. [He Yanfeng, Li Xiujin, Fang Wenjie, Konka is beautiful, NaOH solid-state pretreatment on the impact of cellulosic structure characteristic in straw, regenerative resource, 2007,25 (5): 31.] point out, cellulose is the polysaccharose substance that photosynthesis of plant produces, and is renewable natural resources the abundantest on the earth, and Itzen extrapolates plant in nineteen eighty-three and is equivalent to whole mankind 70kg for each person every day by the cellulose amount of photosynthesis synthesis renewal every year.
Utilize the method for physics or chemical modification to produce and have high value-added product, wherein, blending and modifying is one of important means.Cellulose (Cellulose) fiber is carried out to report a lot [ZengJ, XuX.Y., the ChenXS. of blending and modifying, LiangQ.Z., BianX.C., YangL.X.andJingX.B.Biodegradableelectrospunfibersfordrug delivery [J]. Liu Diansen, Shen Qing, Wang Zhixin, Zhuan Qi, preparation and the sustained release performance of cellulose/polyethylene glycol/vitamin blend film are studied [J], Cellulose Science and technology, 2004,12 (3): 25.Yuan Ye, Fan Ziqian, Shen Qing, nano-cellulose Study and appliance progress I. [J], macromolecule is circulated a notice of, 2010,2:7.ChenG., WangL., LuG..Regeneratedcellulosefiberblendyarn, hasoneoffibersprovidedgreaterthanplantfibere.g.woodpulpf iber, regeneratedcellulosefiber, compositefibere.g.terylenefiber, andproteinfibere.g.rabbitwoolfiber [P] .2008, PN:CN101195940-A.TianS., LiuH., LiuJ., JiangM., LiL., HuangL..Soybeanprotein/alginate/cellulosefibercontainspr esetamountofsoybeanprotein, alginateandcellulosefiber, andhaspresetdrybreakingstrength, drybreakingextendingdegreeandwetmodulus [P] .2008, PN:CN101168869-A.FengT., WangY., LiuY., ChenM..Lignose-bamboocellulosecompositefiberusedformanuf acturingtextiles, suchasclothes, socks, anddecorativecloths, compriseslignoseandbamboocelluloseatspecificweightratio [P] .2008, PN:CN101240455-A.], Donghua University Shen Qing [Wang Zhixin, Shen Qing, Gu Qingfeng, Wang Yimin, containing preparation and the mechanical property [J] of the fiber fabrication & properties research I. persimmon leaf fibre element blended fiber of medicinal herb components, synthetic fiber industry, 2004, 27 (4): 7, Yuan Ye, Fan Ziqian, Shen Qing, nano-cellulose Study and appliance progress I., macromolecule circular [J], 2010,2:7, Zhang Duo, Shen Qing, chemically obtain the progress of regenerative resource from biological material, living beings Chemical Engineering [J], 2010,4 (2): 48.] research group with dimethyl sulfoxide (DMSO) DMSO/ paraformaldehyde (PF) for solvent, add persimmon leaf active component, application wet spinning technology, obtained a kind of regenerated celulose fibre containing extractive from leaves of persimmon.[Zhu Jinzhong, Su Yuheng, Mao Huixian, Yan Guangsong, the moisture pick-up properties of soybean protein/cellulose blending fibre, textile journal, 2010,31 (10): 14 such as Zhu Jinzhong.] report the hygroscopicity of the soybean protein/cellulose blending fibre of different soybean protein blending amount, comparative analysis this fiber and the hygroscopic difference of bamboo fibre, flax and tossa, found that the hygroscopicity of blended fiber improves along with the increase of soy protein content.[Zhang Ruiwen, Zhang Wei, the Structure and Properties of soybean protein/viscose glue blending fiber, Cellulose Science and technology, 2007,15 (2): 49 such as Zhang Ruiwen.] compare the Structure and Properties of soybean protein/viscose glue blending fiber, find that the cross sectional shape of soybean protein/viscose glue blending fiber is similar with common viscose fiber, but surface grooves is more obvious, fiber surface is dispersed with a large amount of protein bodies, makes fiber have good skin-friendly.United States Patent (USP) [publication number US2009166916-A1] gives a kind of method that native cellulose/shitosan two component blend solution prepares composite cellulose fiber, and point out that this fiber can be applied to senior denim fabric [TiChouW., HuangK., LaiM..Processingmethodofnaturalcellulosefiberusedinfor, e.g.forhighclassjeans, involvesmodifyingpropertiesofchitosan, reducingchitosantonanometerbysol-gelmethod, andformingquasi-dopebyprocessingofchitosan [P] .].United States Patent (USP) [publication number US2009088564-A1; US7828936-B2] [LuoM., NeogiAN., WestH..Dissolvingcellulosee.g.woodchipusefulinfiber, involvesmixingcellulosebasedrawmaterialwithmixtureofdipo laraproticintercrystallineswellingagentandionicliquidhav ingspecificmolarratio, atspecifictemperatureandtime [P] .2009] disclose a kind of method of dissolving cellulos.United States Patent (USP) [publication number US2008076313-A1] [UitenbroekD., BlanzJ.J..Wipeforwipinghardsurfacesuchascounter, floor, furniture, tileandceramics, comprisesnonwovensubstratehavingmixtureofnaturalfiberand regeneratedcellulosefiber, andactiveagent-containingcomposition, 2008] propose to prepare with natural fabric and renewable cellulose fibre and active agent intermixture etc. and can wipe clean desk, floor, furniture, ceramic tile, the rag of the objects such as pottery.Japan Patent [publication number JP2009155772-A] [AbeS., HamaguchiY., OgitaN..Manufactureoffinecellulosefiberfor, e.g.substrateforsolarcell, involvesperformingdisentanglementofcellulosesuspensionwh ichisejectedduringpurificationofwoodenmaterialinaqueousm ediumathighvoltage [P] .2009] then give a kind of method preparing high-quality lignocellulose fiber.
Make a general survey of document, in the data reported, have many types to the fiber of cellulose blending modification, but report that the lignocellulose that polymer degree is high is little, and the blending and modifying lignocellulose fiber adding papain is not seen.Papain has the ability of dissolving dead cell, and can the old skin of digest and decompose and do not injure new skin discriminatively, add in cosmetics and can eliminate blackspot, freckle, process slough and scar, have effect [Zhang Wenxue, Hu Cheng that treatment acne increase skin elasticity and beautify skin, Li Shi is strong, the application feature of carica papaya resources, Sichuan food and fermentation, 2000 (1): 26; Liu Si, Shen Wentao, Li little Ying, Zhou Peng, the healthy nutritive value of papaya and product development, guangdong agricultural science, 2007,2:68; Wu Xianrong, the enzyme of papaya and the application in cosmetics thereof, tropical crops science and technology, 1999 (4): 69.]。
Biology enzyme is owing to having the selectivity of height and high efficiency catalytic capability, and non-environmental-pollution, and extensive application is obtained in the biological processing of textiles.In the bioenzyme washing of denim arranges, the treatment effect same with stone mill can be obtained; In surface dressing, can fabric feeling be improved, improve drapability and flexibility; In style arranges, can make Tencel, rayon silk piece goods has peach face outward appearance, cotton fiber has super soft feeling; Can finishing functions be carried out in addition, obtain antibacterial, felt proofing, refuse the effects such as water.In all plant cysteine proteases, papain (papain) family studies the most detailed.Papain (papain) family comprises papain (papain), chymopapain A(ChymopapainA), chymopapain B(ChymopapainB), the multiple protein hydrolase such as pawpaw PEPB B (papayaPeptedaseB).Wherein, papain is extensively present in the root of papaya (Caricapapaya), stem, leaf and fruit, and wherein in immature milk, content is the abundantest.Compared with other cysteine proteinases, papain is comparatively cheap, and has good stability than other alkali protease, therefore has very large using value.Be widely used in food service industry, as the clarification of beer and the tenderization of meat and leather, weaving, daily use chemicals and pharmaceuticals industry.
Along with the development of Science and Technology, the increase of the environmental consciousness idea of people, as green material free from environmental pollution---cellulosic Application Areas also will obtain more wide expansion.Constantly starting in " green " tide, it is by the favor more by people.Under the prerequisite that the current health renewal of ideas, spectrum of disease change, aging society arrive, medical model also by simple disease therapy to prevention, health care future development, and along with transition of China's economy, be of great immediate significance with the research and development of the lignocellulose/papain fiber of biology enzyme blending and modifying.
summary of the invention:
The invention provides a kind of biology enzyme/lignocellulose composite fibre and preparation method thereof, its composite fibre tool health, cosmetology function of producing, carry out wet spinning and electrostatic spinning after adopting even spinning solution blended, effectively can be loaded into cellulose composite fiber and the nano-composite fiber felt of biology enzyme respectively.Compared with traditional cellulose fibre, the standby fiber of Static Spinning legal system has that specific area is large, quality is light.
The preparation method of the present invention's a kind of biology enzyme/lignocellulose composite fibre, comprises the following steps:
(1) prepare homogeneous phase solution, lignocellulose fragment is dissolved in N-ethylpyridine villaumite/boratory dicyandiamide solution of 1-ethyl-3-methylimidazole, form homogeneous phase solution;
(2) prepare co-blended spinning solution, by a certain amount of biology enzyme powder, be dissolved in the homogeneous phase solution described in (1) step, form the heterogeneous Polymer Solution system mixed, be mixed with the co-blended spinning solution mixed;
(3) spinning solution processed, obtains spinning solution by the co-blended spinning solution deaeration described in (2) step, filtration;
(4) spin biology enzyme/lignocellulose composite fibre, adopt wet spinning or electrostatic spinning technique (3) step spinning solution to be spun into the composite fibre of year biology enzyme/lignocellulose, and rinsing, drying are carried out to it, dehumidify to obtain product.
The preparation method of a kind of biology enzyme/lignocellulose composite fibre of the present invention, preferably as follows:
(1) prepare homogeneous phase solution, lignocellulose fragment is dissolved in the boratory ionic liquid mixed solvent system of N-ethylpyridine villaumite/1-ethyl-3-methylimidazole, form homogeneous phase solution;
(2) prepare co-blended spinning solution, by a certain amount of biology enzyme powder under room temperature, be dissolved in the homogeneous phase solution described in (1) step, form the heterogeneous Polymer Solution system mixed, be mixed with the co-blended spinning solution mixed;
(3) spinning solution processed, obtains spinning solution by the co-blended spinning solution deaeration described in (2) step, filtration under room temperature;
(4) biology enzyme/lignocellulose composite fibre is spinned, wet spinning or electrostatic spinning technique is adopted under room temperature, by (3) step spinning solution, be spun into the composite fibre or nano-composite fiber felt that carry biology enzyme/lignocellulose, and rinsing is first carried out to it to be placed in air naturally dry or low temperature drying dehumidifying in vacuum drying oven, obtain product.
Step of the present invention (1) control N-ethylpyridine villaumite and the boratory quality mol ratio of 1-ethyl-3-methylimidazole are 1.00-7.59; The degree of polymerization of lignocellulose is 600-2000, and lignocellulose fragment solution temperature is 60 DEG C-120 DEG C, and in homogeneous phase solution, the quality hundred of lignocellulose is than being 8.00%-15.00%.
Biology enzyme of the present invention be in papain, chymopapain A, chymopapain B, pawpaw PEPB B any one.
The mass concentration controlling biology enzyme in co-blended spinning solution in described step (2) is 0.01%-8.33%.
Described step (4) wet spinning condition is: the time controlling sealing and standing deaeration in material-storage jar is 1.0-2.0 hour; Pressure in material-storage jar is 1.5 × 10
5pa; Coagulation bath temperature is 10
oc-30
oc; The bath temperature of desolvation is 20
oc ~ 40
oc; The temperature that the boiling water bath of desolvation stretches is 90
oc-100
oc; After winding, the compacting by drying temperature of fiber is 30
oc-60
oc; The fibre single thread fiber number of spinning is 2.2dtex-3.2dtex, intensity is 0.9cN/dtex-2.8cN/dtex.
Step of the present invention (4) electrospinning conditions is: in syringe, spinning solution flow velocity is 0.7-1.5mL/h, and the voltage applied is 12-14kV, and two interpolar screen needle gages are 14-19cm; The baking temperature of the nano-composite fiber felt of spinning is 30 DEG C-60 DEG C, and drying time is 3-5 hour.
A kind of biology enzyme/lignocellulose composite fibre prepares according to upper described method.
The present invention first has bioactive ingredients papain, degradable natural polymer miscible environment-friendly type solvent compartment temperature ionic liquid [Wang Huaping with including, Zhang Yumei etc., a kind of ionic liquid is the recovery method of solvent in the cellulose fibre preparation of solvent, number of patent application: 200510111966.3, take ionic liquid as the method that cellulose fibre prepared by solvent, number of patent application: 200610026709.4] middle preparation homogeneous phase spinning solution, adopt wet spinning process and method of electrostatic spinning to prepare year enzyme fiber respectively.Wherein wet spinning fiber can become fabric by textile process further, and finally can make a year enzyme textiles, as underwear, brassiere, socks, shoes, bady's diaper etc., make bioenzyme activity composition slow releasing from cloth fibers, the contact of people just by skin and dress material in daily donning process completes the process with enzyme beautifying skin, thus meets biology enzyme contact comprehensively and exempt the trouble of the every daily skin care products of people; Then local beauty etc. is more suitable for the enzyme fiber that carries that Electrospinning Method obtains.
The composite fiber product utilizing the inventive method to prepare has following beneficial effect:
(1) compared with popular cellulosic fibre material, spin out biology enzyme papain/lignocellulose composite fibre and health textiles thereof, can occur by effective beautifying skin, complied with the development trend that current treatment medical science turns to physical-fitness medicine; The application of wet spinning technology, is conducive to improving spinning speed, improves product mechanical property and production efficiency;
(2) electrostatic spinning technique spins out biology enzyme papain/lignocellulose composite nano fiber and has the advantages such as quality is light, specific area is large, wearing comfort, convenient;
(3) two classes more than carry biology enzyme fiber or textiles is applicable to colony's beauty treatment skin, are a kind of novel containing biology enzyme papain carrier model fiber and a kind of grade textiles, as eyeshade, mouth mask, brassiere, underwear etc.;
(4) dress ornament that improve product is comfortable, health, improves fibre property, adds added value of product, while raising people's living standard, increase huge economic benefit.
detailed description of the invention:
Below in conjunction with detailed description of the invention, the present invention is further elaborated.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
The present invention as follows step carries out: (1) preparation dicyandiamide solution is N-ethylpyridine villaumite ([bmim] Cl)/1-ethyl-3-methylimidazole borate ([bmim] [BF
4]) ionic liquid at room temperature mixed solvent, lignocellulose fragment is dissolved in above-mentioned dicyandiamide solution and forms homogeneous phase solution;
(2) take a certain amount of biology enzyme papain powder under room temperature, be dissolved in the solution described in (1), form the heterogeneous Polymer Solution system mixed, be mixed with the co-blended spinning solution mixed;
(3) under room temperature, the deaeration of described to (2) formation homogeneous phase solution mixed system, filtration are obtained spinning solution;
(4) adopt wet spinning technology to spin the composite fibre carrying papain under room temperature, the fiber rinsing of spinning is placed on naturally dry in air or low temperature drying dehumidifying in vacuum drying oven;
(5) adopt electrostatic spinning technique to spin the nano-composite fiber felt carrying papain under room temperature, the nanofiber mats of spinning is placed in vacuum drying oven low temperature drying dehumidifying.
N-ethylpyridine villaumite ([bmim] Cl)/1-ethyl-3-methylimidazole borate ([bmim] [BF in described step (1)
4]) mol ratio of ionic liquid at room temperature is between 1.00-7.59; The degree of polymerization of lignocellulose is between 600-2000, and lignocellulose fragment solution temperature is between 60 DEG C-120 DEG C, and in solution system, lignocellulose mass percent is 8.00%-15.00%.
Described step (2) biological enzyme comprises following any one:
Papain (papain), chymopapain A(ChymopapainA), chymopapain B(ChymopapainB), the multiple protein hydrolase such as pawpaw PEPB B (papayaPeptedaseB).
The mass percent of described step (2) biology enzyme is greater than 0.01% and is less than or equal to 8.33%.
Described step (4) wet spinning condition is: in material-storage jar, the time of sealing and standing deaeration is about 1.0-2.0 hour; Open air compressor, the constant pressure kept in material-storage jar is 1.5 × 10
5pa; Coagulating bath is 0.1%-60% ionic liquid at room temperature---the deionized water solution with the same solvent composition adopted in spinning solution; Coagulation bath temperature is 10
oc-30
oc; The predraft bath temperature that can remove partial solvent is 20
oc-40
oc; The temperature that further desolvation boiling water bath stretches is 90
oc-100
oc; After winding, the compacting by drying temperature of fiber is 30
oc-60
oc; The fibre single thread fiber number of spinning is 2.2dtex-3.2dtex, intensity is 0.9cN/dtex-2.8cN/dtex.
Described step (5) electrospinning conditions is: in syringe, spinning solution flow velocity is 0.7-1.5mL/h, and the voltage applied is 12-14kV, and two interpolar screen needle gages are 14-19cm; The baking temperature of the nanofiber mats of spinning is between 30 DEG C-60 DEG C, and drying time is 3-5 hour.
embodiment 1
Raw material: papain, rank is 6U/mg; Lignocellulose fragment, the degree of polymerization
=1800, N-ethylpyridine villaumite ([bmim] Cl) and 1-ethyl-3-methylimidazole borate ([bmim] [BF
4]) all adopt analysis pure;
Lignocellulose thickness being about 0.1-0.5cm is cut into fragment, 100
oin the vacuum drying oven of C, about 6hrs that is 6 hours, reaches the cellulosic object of removal moisture drying.The 1-ethyl-3-methylimidazole borate of 154.15gN-ethylpyridine villaumite and 60.80g is taken separately with the beaker of 100mL, add in the three-necked bottle that the excellent also 250-mL of good seal of mechanical agitation is housed, and the silicone oil bath this bottle is placed in heat insulation and heating equipment, control to remain on 90 when oil bath temperature starts
oc.Take dried lignocellulose 23.90g, a sealing-plug of three-necked bottle of back-outing, joins disposable for lignocellulose in three-necked bottle, and then good seal, for making each bottle environment be consistent, interval is opened and is connected vacuum extractor, to keep the dissolving environment in bottle.Observe that to stir continuously lignocellulose after 1.5 hours all swelling, perusal, less than obvious fragment, makes homogeneous phase solution.Turn off heater, etc. the temperature of system from 110
oc is reduced to 60
oduring C, take 5.87g papain and add in three-necked bottle, make co-blended spinning solution.
By the spinning solution of above-mentioned preparation, filter and deaeration etc. delivers to spinning machine after preparing before spinning, and measured by Spinning pumps, enter spinning head through candle filter, gooseneck, the solution thread extruded from spinneret capillary enters coagulating bath, forms fiber.Spinning solution is from material-storage jar after measuring pump metering supercharging, and clamp-on coagulating bath from spinnerets, the coagulating bath adopted here is volume content is 30%, mixed at room temperature ionic liquid-deionized water solution, and temperature is 16
oc; The tow after solidification that is shaped is walked around the first deflector roll and is entered temperature and be about 25
othe predraft water-bath of C also removes partial solvent, walks around the second deflector roll and carries out predraft; Tow enters boiling water bath and carries out boiling water bath and stretch and to go forward side by side one-step removal solvent afterwards, and the temperature that boiling water bath stretches is 90
oc-100
oc; By winding, drafting multiple is wherein set and equals 6; Winding speed is 20 ms/min; After the fiber rinsed with deionized water that collection has spinned 3 times, in 30
opreserve after carrying out compacting by drying under C, object be the residual solvent of removing and moisture in case below at testing and analysis.Sample (a) filament number finally obtained is 2.8dtex, intensity 1.9cN/dtex, and sample (b) filament number is 3.2dtex, intensity 2.3cN/dtex.Sample (a) and sample (b) are the biology enzyme papain/lignocellulose composite fiber product of two kinds of filament numbers.
embodiment 2
Raw material: papain, rank is 6U/mg; Lignocellulose fragment, the degree of polymerization
=1800, N-ethylpyridine villaumite ([bmim] Cl) and 1-ethyl-3-methylimidazole borate ([bmim] [BF4]) are all analyze pure rank.
Lignocellulose thickness being about 0.1-0.5cm is cut into fragment about 6hrs in the vacuum drying oven of 100 DEG C, reaches the cellulosic object of removal moisture drying.The 1-ethyl-3-methylimidazole borate of 154.15gN-ethylpyridine villaumite and 60.80g is taken separately with the beaker of 100mL, add in the three-necked bottle that the excellent also 250-mL of good seal of mechanical agitation is housed, and the silicone oil bath this bottle is placed in heat insulation and heating equipment, control to remain on 90 when oil bath temperature starts
oc.Take dried lignocellulose 23.90g, a sealing-plug of three-necked bottle of back-outing, joins in three-necked bottle disposable for lignocellulose, and then good seal, and interval is opened and connected vacuum extractor, to keep the dissolving environment in bottle.Observe that to stir continuously lignocellulose after 1.5 hours all swelling, perusal is less than obvious fragment.Turn off heater, etc. the temperature of system from 110
oc is reduced to 60
oduring C, taking 5.87g papain, to add mass percent in three-necked bottle be 2.40%.Continue after adding to stir, open firing equipment, keep oil bath temperature to be 60
oc.
The spinning solution of above-mentioned preparation is respectively charged into the syringe of 5mL, injection needle is tack, and internal diameter is 0.45mm, connects the positive pole of high pressure generator, and aluminium foil receiving screen connects negative pole, for receiving electrostatic spinning fiber.According to preliminary result, being set as follows of each parameter of spinning process: the flow velocity of solution at spinning nozzle place is 1.0mL/h, the voltage applied is 12kV, and two interpolar screen needle gages are 19cm, operate under room temperature.Under high voltage electric field effect, spinning solution sprays the final fiber laydown that formed on receiving screen, forms tunica fibrosa.Tunica fibrosa is placed in 40
oCdried overnight in vacuum drying chamber, to remove residual solvent and moisture.
The diameter span of electrospun composite fibers is that the diameter of (a-pure cellulose) electrospinning fibre is respectively 290 ± 209 and (b-carries enzyme-cellulose) 262 ± 102nm.
Claims (7)
1. a preparation method for biology enzyme/lignocellulose composite fibre, comprises the following steps:
(1) prepare homogeneous phase solution, lignocellulose fragment is dissolved in N-ethylpyridine villaumite/boratory dicyandiamide solution of 1-ethyl-3-methylimidazole, form homogeneous phase solution;
(2) prepare co-blended spinning solution, by a certain amount of biology enzyme powder, be dissolved in the homogeneous phase solution described in (1) step, form the heterogeneous Polymer Solution system mixed, be mixed with co-blended spinning solution;
(3) spinning solution processed, obtains spinning solution by the co-blended spinning solution deaeration described in (2) step, filtration;
(4) biology enzyme/lignocellulose composite fibre is spinned, adopt wet spinning or electrostatic spinning technique by (3) step spinning solution, be spun into and carry the composite fibre of biology enzyme/lignocellulose or nano-composite fiber felt, and rinsing, drying are carried out to it, dehumidify to obtain product;
Described biology enzyme be in papain, chymopapain A, chymopapain B, pawpaw PEPB B any one.
2., according to the preparation method of a kind of biology enzyme/lignocellulose composite fibre according to claim 1, it is characterized in that comprising the following steps:
(1) prepare homogeneous phase solution, lignocellulose fragment is dissolved in the boratory ionic liquid mixed solvent system of N-ethylpyridine villaumite/1-ethyl-3-methylimidazole, form homogeneous phase solution;
(2) prepare co-blended spinning solution, by a certain amount of biology enzyme powder under room temperature, be dissolved in the homogeneous phase solution described in (1) step, form the heterogeneous Polymer Solution system mixed, be mixed with the co-blended spinning solution mixed;
(3) spinning solution processed, obtains spinning solution by the co-blended spinning solution deaeration described in (2) step, filtration under room temperature;
(4) biology enzyme/lignocellulose composite fibre is spinned, wet spinning or electrostatic spinning technique is adopted under room temperature, by (3) step spinning solution, be spun into the composite fibre or nano-composite fiber felt that carry biology enzyme/lignocellulose, and after first rinsing is carried out to it, be placed in air air dry or in vacuum drying oven low temperature drying dehumidifying, obtain product.
3., according to the preparation method of a kind of biology enzyme/lignocellulose composite fibre described in claim 1 or 2, it is characterized in that described step (1) control N-ethylpyridine villaumite and the boratory mol ratio of 1-ethyl-3-methylimidazole are 1.00-7.59; The degree of polymerization of lignocellulose is 600-2000, and lignocellulose fragment solution temperature is 60 DEG C-120 DEG C, and in homogeneous phase solution, the mass percent of lignocellulose is 8.00%-15.00%.
4., according to the preparation method of a kind of biology enzyme/lignocellulose composite fibre described in claim 1 or 2, it is characterized in that the mass concentration controlling biology enzyme in co-blended spinning solution in described step (2) is 0.01%-8.33%.
5. according to the preparation method of a kind of biology enzyme/lignocellulose composite fibre described in claim 1 or 2, it is characterized in that described step (4) wet spinning condition is: the time controlling sealing and standing deaeration in material-storage jar is 1.0-2.0 hour; Pressure in material-storage jar is 1.5 × 10
5pa; Coagulation bath temperature is 10
oc-30
oc; The bath temperature of desolvation is 20
oc-40
oc; The temperature that the boiling water bath of desolvation stretches is 90
oc-100
oc; After winding, the compacting by drying temperature of fiber is 30
oc-60
oc; The fibre single thread fiber number of spinning is 2.2dtex-3.2dtex, intensity is 0.9cN/dtex-2.8cN/dtex.
6. according to the preparation method of a kind of biology enzyme/lignocellulose composite fibre described in claim 1 or 2, it is characterized in that described step (4) electrospinning conditions is: in syringe, spinning solution flow velocity is 0.7-1.5mL/h, the voltage applied is 12-14kV, and two interpolar screen needle gages are 14-19cm; The baking temperature of the nano-composite fiber felt of spinning is 30 DEG C-60 DEG C, and drying time is 3-5 hour.
7. biology enzyme/lignocellulose the composite fibre prepared according to the method described in claim 1 or 2.
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| CN101934086A (en) * | 2009-07-02 | 2011-01-05 | 胡平 | Formula of electrostatic spinning raw material solution for tissue repairing |
| CN101982578A (en) * | 2010-08-13 | 2011-03-02 | 湖南金鹰服饰集团有限公司 | Method for preparing lignocellulose fibers |
| CN102517689A (en) * | 2011-12-02 | 2012-06-27 | 华南理工大学 | Lignin base skin core structure nanometer/micron fiber and preparation method thereof |
| CN102716684A (en) * | 2012-07-06 | 2012-10-10 | 北京师范大学 | Method for eutrophic water pollution treatment through polylactic acid fiber membrane immobilized compound enzyme technology |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101934086A (en) * | 2009-07-02 | 2011-01-05 | 胡平 | Formula of electrostatic spinning raw material solution for tissue repairing |
| CN101982578A (en) * | 2010-08-13 | 2011-03-02 | 湖南金鹰服饰集团有限公司 | Method for preparing lignocellulose fibers |
| CN102517689A (en) * | 2011-12-02 | 2012-06-27 | 华南理工大学 | Lignin base skin core structure nanometer/micron fiber and preparation method thereof |
| CN102716684A (en) * | 2012-07-06 | 2012-10-10 | 北京师范大学 | Method for eutrophic water pollution treatment through polylactic acid fiber membrane immobilized compound enzyme technology |
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