CN104032400A - Biological enzyme/lignocellulose composite fiber and preparation method thereof - Google Patents
Biological enzyme/lignocellulose composite fiber and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a biological enzyme/lignocellulose composite fiber and a preparation method thereof. The preparation method comprises the steps of (1) dissolving lignocellulose fragments into N-ethyl pyridine chloride salt ((bmim) Cl)/1-ethyl-3-methyl imidazole borate ((bmin) (BF4)) mixed ionic liquid at room temperature to form a homogeneous solution; (2) dissolving papain powder into the solution prepared in the step (1) according to certain mass percent to obtain homogeneous mixed spinning dope; and (3) deforming, filtering and metering the spinning dope, and extruding the product by a spinning nozzle to form spinning trickle, enabling the spinning trickle to enter coagulating bath, forming by coagulating, blending the product with the uniform spinning dope, and carrying out wet spinning and electrostatic spinning. The method has the advantages of being environmentally friendly, low in cost, high in spinning speed, high in production efficiency and the like; compared with a traditional textile fiber material, the prepared composite fiber has the advantages of being comfortable, high in yield and the like, can be spun and processed to obtain a fabric, and can be finally prepared into a textile fabric, such as underclothes, a bra, socks and baby diapers, which is loaded with biological enzyme and is capable of beautifying the skin.
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 have experienced semicentennial fast development, the reality that simultaneous petroleum resources are in short supply and environmental protection pressure increases, and 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 that photosynthesis by plant forms, and people are referred to as " green material ".That the reproducible living resources of this class can be described as is inexhaustible, it is applicable to various practical application, has slowed down widely the environmental pollution of asking for He thus causing of the mankind to mineral resources.Especially in current environmental pollution, become in the large atmosphere of mankind's focus, cellulose base material causes people's concern more, has irreplaceable critical role in national economy and daily life.
Native cellulose fibre mainly comes from string, and people utilize the cellulose fibre history of existing several thousand, as fibers such as cotton, fiber crops, timber, bamboos.Cellulose base 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.Its three major polymers: cellulose, hemicellulose and lignin form, and cellulose and hemicellulose are generically and collectively referred to as holocellulose.Lignin, cellulose and hemicellulose are the main components that forms plant skeleton.He Yanfeng etc. [He Yanfeng, Li Xiujin, Fang Wenjie, Konka is beautiful, the impact of NaOH solid-state pretreatment on 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, Itzen extrapolates in nineteen eighty-three the cellulose amount that plant synthesize renewal by photosynthesis every year and is equivalent to the whole mankind 70 kg for each person every day.
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 [Zeng J, Xu X.Y., the Chen X S. of blending and modifying, Liang Q. Z., Bian X. C., Yang L. X. and Jing X. B. Biodegradable electrospun fibers for drug delivery[J]. Liu Diansen, Shen Qing, Wang Zhixin, Zhuan Qi, the preparation of cellulose/polyethylene glycol/vitamin blend film and sustained release performance research [J], Cellulose Science and technology, 2004,12 (3): 25.Yuan Ye, Fan Ziqian, Shen Qing, nano-cellulose research and application progress I. [J], macromolecule circular, 2010,2:7.Chen G., Wang L., Lu G.. Regenerated cellulose fiber blend yarn, has one of fibers provided greater than plant fiber e.g. wood pulp fiber, regenerated cellulose fiber, composite fiber e.g. terylene fiber, and protein fiber e.g. rabbit wool fiber[P]. 2008, PN:CN101195940-A. Tian S., Liu H., Liu J., Jiang M., Li L., Huang L.. Soybean protein/alginate/cellulose fiber contains preset amount of soybean protein, alginate and cellulose fiber, and has preset dry breaking strength, dry breaking extending degree and wet modulus[P]. 2008, PN:CN101168869-A. Feng T., Wang Y., Liu Y., Chen M.. Lignose-bamboo cellulose composite fiber used for manufacturing textiles, such as clothes, socks, and decorative cloths, comprises lignose and bamboo cellulose at specific weight ratio[P]. 2008, PN:CN101240455-A.], Shen Qing [the Wang Zhixin of Donghua University, Shen Qing, Gu Qingfeng, Wang Yimin, containing the fiber preparation of medicinal herb components and preparation and the mechanical property [J] of performance study I. persimmon leaf fibre element blended fiber, synthetic fiber industry, 2004, 27 (4): 7, Yuan Ye, Fan Ziqian, Shen Qing, nano-cellulose research and application progress I., macromolecule circular [J], 2010,2:7, Zhang Duo, Shen Qing, obtains the progress of regenerative resource, living beings Chemical Engineering [J], 2010,4 (2): 48 from biological material by chemical method.] research group to take dimethyl sulfoxide (DMSO) DMSO/ paraformaldehyde (PF) be solvent, add persimmon leaf active component, application wet spinning technology, has made 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.] reported 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 of soybean protein/viscose glue blending fiber and performance, Cellulose Science and technology, 2007,15 (2): 49 such as Zhang Ruiwen.] compared structure and the performance of soybean protein/viscose glue blending fiber, the cross sectional shape of finding 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] has provided a kind of method that native cellulose/shitosan two component blend solutions are prepared composite cellulose fiber, and point out that this fiber can be applied to senior denim fabric [Ti Chou W., Huang K., Lai M.. Processing method of natural cellulose fiber used in for, e.g. for high class jeans, involves modifying properties of chitosan, reducing chitosan to nanometer by sol-gel method, and forming quasi-dope by processing of chitosan[P] .].United States Patent (USP) [publication number US2009088564-A1; US7828936-B2] [Luo M., Neogi A N., West H.. Dissolving cellulose e.g. wood chip useful in fiber, involves mixing cellulose based raw material with mixture of dipolar aproticintercrystalline swelling agent and ionic liquid having specific molar ratio, at specific temperature and time[P]. 2009] a kind of method of dissolving cellulos disclosed.United States Patent (USP) [publication number US2008076313-A1] [Uitenbroek D., Blanz J. J.. Wipe for wiping hard surface such as counter, floor, furniture, tile and ceramics, comprises nonwoven substrate having mixture of natural fiber and regenerated cellulose fiber, and active agent-containing composition, 2008] proposed to prepare and can wipe clean desk with natural fabric and renewable cellulose fibre and active agent intermixture etc., floor, furniture, ceramic tile, the rag of the objects such as pottery.Japan Patent [publication number JP2009155772-A] [Abe S., Hamaguchi Y., Ogita N.. Manufacture of fine cellulose fiber for, e.g. substrate for solar cell, involves performing disentanglement of cellulose suspension which is ejected during purification of wooden material in aqueous medium at high voltage[P]. 2009] provided a kind of method of preparing high-quality lignocellulose fiber.
Make a general survey of document, in the data of having reported, the fiber of cellulose blending modification is had to many types, but the high lignocellulose of report polymer degree seldom, and add the blending and modifying lignocellulose fiber of papain not see.Papain has the ability of dissolving dead cell, and 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, [Zhang Wenxue, holds recklessly with the effect of beautifying skin to have treatment acne increase skin elasticity, Li Shi is strong etc., 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 selectivity and the high efficiency catalytic capability of height, and non-environmental-pollution, and has obtained extensive application in the biological processing of textiles.In the bioenzyme washing of denim arranges, can obtain the treatment effect same with stone mill; In surface dressing, can improve fabric feeling, improve drapability and flexibility; In style arranges, can make Tencel, rayon silk piece goods there is peach face outward appearance, cotton fiber has super soft feeling; Can carry out finishing functions in addition, obtain antibacterial, felt proofing, refuse water texts.In all plant cysteine proteinases, papain (papain) family studies the most detailedly.Papain (papain) family comprises papain (papain), chymopapain A(Chymopapain A), chymopapain B(Chymopapain B), the multiple protein hydrolase such as pawpaw PEPB B (papaya Peptedase B).Wherein, papain is extensively present in the root, stem, leaf and fruit of papaya (Carica papaya), and wherein in immature milk, content is the abundantest.Compare 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 tenderization of the clarification of beer and meat and leather, weaving, daily use chemicals and pharmaceuticals industry.
Along with the development of Science and Technology, the increase of people's environmental consciousness idea, as green material free from environmental pollution---cellulosic Application Areas also will obtain more wide expansion.In constantly starting " green " tide, it will more be subject to people's favor.Under the prerequisite that current concept of health upgrades, spectrum of disease changes, aging society arrives, medical model also by simple treatment disease to prevention, health care future development, and along with the transition of China's economy, with the research and development of lignocellulose/papain fiber of biology enzyme blending and modifying, be of great immediate significance.
summary of the invention:
The invention provides a kind of biology enzyme/lignocellulose composite fibre and preparation method thereof, the composite fibre tool health of its production, cosmetology function, after adopting even spinning solution blend, carry out wet spinning and electrostatic spinning, can obtain respectively being effectively written into cellulose composite fiber and the nano-composite fiber felt of biology enzyme.Compare 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 a kind of biology enzyme/lignocellulose of the present invention composite fibre, comprises the following steps:
(1) preparation homogeneous phase solution, is dissolved in lignocellulose fragment in the boratory dicyandiamide solution of N-ethylpyridine villaumite/1-ethyl-3-methylimidazole, forms homogeneous phase solution;
(2) preparation co-blended spinning solution, by a certain amount of biology enzyme powder, is dissolved in the homogeneous phase solution described in (1) step, forms the heterogeneous Polymer Solution system mixing, and is mixed with the co-blended spinning solution mixing;
(3) spinning solution processed, obtains spinning solution by the co-blended spinning solution deaeration described in (2) step, filtration;
(4) spinning biology enzyme/lignocellulose composite fibre, adopts wet spinning or electrostatic spinning technique will (3) step spinning solution to be spun into the composite fibre of year biology enzyme/lignocellulose, and to its carry out rinsing, product is dried, dehumidifies and to obtain.
The preparation method of a kind of biology enzyme/lignocellulose composite fibre of the present invention, preferably as follows:
(1) preparation homogeneous phase solution, is dissolved in lignocellulose fragment in the boratory ionic liquid mixed solvent system of N-ethylpyridine villaumite/1-ethyl-3-methylimidazole, forms homogeneous phase solution;
(2) preparation co-blended spinning solution, by a certain amount of biology enzyme powder, is dissolved in the homogeneous phase solution described in (1) step under room temperature, forms the heterogeneous Polymer Solution system mixing, and is mixed with the co-blended spinning solution mixing;
(3) spinning solution processed, obtains spinning solution by the co-blended spinning solution deaeration described in (2) step, filtration under room temperature;
(4) spinning biology enzyme/lignocellulose composite fibre, under room temperature, adopt wet spinning or electrostatic spinning technique, by (3) step spinning solution, be spun into the composite fibre or the nano-composite fiber felt that carry biology enzyme/lignocellulose, and it is first carried out to rinsing be placed in air naturally dry or low temperature drying dehumidifying in vacuum drying oven, obtain product.
Step of the present invention (1) is controlled N-ethylpyridine villaumite and the boratory quality mol ratio of 1-ethyl-3-methylimidazole is 1.00-7.59; The degree of polymerization of lignocellulose is 600-2000, and lignocellulose fragment solution temperature is 60 ℃-120 ℃, 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 of 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 of 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 reeling, the compacting by drying temperature of fiber is 30
oc-60
oc; The fibre single thread fiber number of spinning is that 2.2dtex-3.2dtex, intensity are 0.9 cN/dtex-2.8cN/dtex.
Step of the present invention (4) electrostatic spinning condition is: in syringe, spinning solution flow velocity is 0.7-1.5 mL/h, and the voltage applying is 12-14 kV, and two interpolar screen needle gages are 14-19 cm; The baking temperature of the nano-composite fiber felt of spinning is 30 ℃-60 ℃, and be 3-5 hour drying time.
A kind of biology enzyme/lignocellulose composite fibre prepares according to the method for the above.
The present invention first has bioactive ingredients papain with including, the miscible environment-friendly type of the degradable natural polymer temperature ionic liquid [Wang Huaping of solvent compartment, Zhang Yumei etc., a kind of ionic liquid is the recovery method of solvent in prepared by the cellulose fibre of solvent, number of patent application: 200510111966.3, the ionic liquid of take is prepared the method for cellulose fibre as solvent, number of patent application: 200610026709.4] middle preparation homogeneous phase spinning solution, adopt respectively wet spinning process and method of electrostatic spinning to prepare a year enzyme fiber.Wherein wet spinning fiber further textile process become fabric, and finally can make and carry an enzyme textiles, as underwear, brassiere, socks, shoes, bady's diaper etc., bioenzyme activity composition is slowly discharged from cloth fibers, people just can be by skin in daily wearing process the process of beautifying skin with enzyme that contacted with dress material, thereby meet biology enzyme contact comprehensively and the trouble of exempting the every daily skin care products of people; The enzyme fiber that carries obtaining with Electrospinning Method is more suitable for local beauty etc.
Utilize composite fibre product prepared by the inventive method to there is following beneficial effect:
(1) compare with popular cellulosic fibre material, spin out biology enzyme papain/lignocellulose composite fibre and health textiles thereof, can effectively beautify skin and occur, complied with the development trend that current treatment medical science turns to physical-fitness medicine; The application of wet spinning technology, is conducive to improve 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, and it is comfortable, convenient to dress;
(3) above two classes are carried biology enzyme fiber or textiles is applicable to colony's beauty treatment skin, are a kind of novel biology enzyme papain carrier model fiber and a kind of grade textiles of containing, as eyeshade, mouth mask, brassiere, underwear etc.;
(4) improved that the dress ornament of product is comfortable, health, improved fibre property, increased added value of product, when improving people's living standard, increased huge economic benefit.
the specific embodiment:
Below in conjunction with the specific embodiment, the present invention is further elaborated.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
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) under room temperature, take a certain amount of biology enzyme papain powder, be dissolved in (1) described solution, form the heterogeneous Polymer Solution system mixing, be mixed with the co-blended spinning solution mixing;
(3) under room temperature, the deaeration of (2) described formation homogeneous phase solution mixed system, filtration are obtained to spinning solution;
(4) under room temperature, adopt wet spinning technology spinning to carry the composite fibre of papain, the fiber rinsing of spinning is placed on to naturally dry in air or low temperature drying dehumidifying in vacuum drying oven;
(5) under room temperature, adopt electrostatic spinning technique spinning to carry the nano-composite fiber felt of papain, the nanofiber mats of spinning is placed in to 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 ℃-120 ℃, and in solution system, lignocellulose mass percent is 8.00%-15.00%.
The biological enzyme of described step (2) comprises following any:
Papain (papain), chymopapain A(Chymopapain A), chymopapain B(Chymopapain B), the multiple protein hydrolase such as pawpaw PEPB B (papaya Peptedase B).
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: about 1.0-2.0 hour of the time of sealing and standing deaeration in material-storage jar; Open air compressor, the constant pressure keeping in material-storage jar is 1.5 * 10
5pa; Coagulating bath for spinning solution in 0.1%-60% ionic liquid at room temperature---the deionized water solution of the same solvent composition that adopts; 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 reeling, the compacting by drying temperature of fiber is 30
oc-60
oc; The fibre single thread fiber number of spinning is that 2.2dtex-3.2dtex, intensity are 0.9 cN/dtex-2.8cN/dtex.
Described step (5) electrostatic spinning condition is: in syringe, spinning solution flow velocity is 0.7-1.5 mL/h, and the voltage applying is 12-14 kV, and two interpolar screen needle gages are 14-19 cm; The baking temperature of the nanofiber mats of spinning is between 30 ℃-60 ℃, and be 3-5 hour drying time.
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;
The lignocellulose of the about 0.1-0.5cm of thickness is cut into fragment, 100
oin the vacuum drying oven of C, about 6hrs is 6 hours, reaches the cellulosic object of removal moisture drying.With the beaker of 100mL, take separately the 1-ethyl-3-methylimidazole borate of 154.15g N-ethylpyridine villaumite and 60.80g, add in the three-necked bottle of the 250-mL that mechanical agitation rod good seal are housed, and this bottle is placed in to the silicone oil bath with heat insulation and heating equipment, control when oil bath temperature starts and remain on 90
oc.Take dried lignocellulose 23.90g, a sealing-plug of the three-necked bottle of back-outing, joins in three-necked bottle lignocellulose is disposable, and then good seal, for each bottle of environment is consistent, interval is opened and is connected vacuum extractor, to keep the dissolving environment in bottle.Observe continuous stirring whole swellings of lignocellulose after 1.5 hours, perusal, less than obvious fragment, is made homogeneous phase solution.Turn off heater, etc. the temperature of system from 110
oc is reduced to 60
oduring C, take 5.87 g papains and add in three-necked bottle, make co-blended spinning solution.
By the spinning solution of above-mentioned preparation, after spinning front preparation, filter and deaeration etc. deliver to spinning machine, by Spinning pumps, measure, through candle filter, gooseneck, enter spinning head, the solution thread of extruding from spinneret capillary enters coagulating bath, forms fiber.Spinning solution, is clamp-oned coagulating bath from spinnerets from material-storage jar after measuring pump metering supercharging, and the coagulating bath adopting is here that volume content is 30%, mixed at room temperature ionic liquid-deionized water solution, and temperature is 16
oc; Tow after be shaped solidifying 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 the boiling water bath one-step removal solvent of going forward side by side that stretches afterwards, and the temperature that boiling water bath stretches is 90
oc-100
oc; By coiling, drafting multiple is wherein set and equals 6; Winding speed is 20 ms/min; The fiber that collection has spinned is with after rinsed with deionized water 3 times, in 30
ounder C, carry out preserving after compacting by drying, object be remove residual solvent and moisture in case below in test and analyze.The sample finally obtaining (a) filament number 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 biology enzyme papain/lignocellulose composite fibre 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 to analyze pure rank.
The lignocellulose of the about 0.1-0.5cm of thickness is cut into fragment about 6hrs in the vacuum drying oven of 100 ℃, reaches the cellulosic object of removal moisture drying.With the beaker of 100mL, take separately the 1-ethyl-3-methylimidazole borate of 154.15g N-ethylpyridine villaumite and 60.80g, add in the three-necked bottle of the 250-mL that mechanical agitation rod good seal are housed, and this bottle is placed in to the silicone oil bath with heat insulation and heating equipment, control when oil bath temperature starts and remain on 90
oc.Take dried lignocellulose 23.90g, a sealing-plug of the three-necked bottle of back-outing, joins in three-necked bottle lignocellulose is disposable, and then good seal, and interval is opened and connected vacuum extractor, to keep the dissolving environment in bottle.Observe continuous stirring whole swellings of lignocellulose after 1.5 hours, perusal is less than obvious fragment.Turn off heater, etc. the temperature of system from 110
oc is reduced to 60
oduring C, taking 5.87 g papains, to add mass percent in three-necked bottle be 2.40%.Add and continue afterwards to stir, open firing equipment, keeping oil bath temperature is 60
oc.
The spinning solution of above-mentioned preparation is respectively charged into the syringe of 5 mL, injection needle is tack, and internal diameter is 0.45 mm, connects the positive pole of high pressure generator, and aluminium foil receiving screen connects negative pole, for receiving electrostatic spinning fiber.According to preliminary experiment result, being set as follows of each parameter of spinning process: solution is 1.0 mL/h at the flow velocity at spinning nozzle place, and the voltage applying is 12 kV, two interpolars screen needle gages are 19 cm, under room temperature, operate.Under high voltage electric field effect, spinning solution sprays the final fiber laydown that forms on receiving screen, forms tunica fibrosa.Tunica fibrosa is placed in to 40
oCdried overnight in vacuum drying chamber, to remove residual solvent and moisture.
The diameter span of electrostatic spinning composite fibre is respectively 290 ± 209 and (b-carries enzyme-cellulose) 262 ± 102 nm for the diameter of (a-pure cellulose) electrospinning fibre.
Claims (8)
1. a preparation method for biology enzyme/lignocellulose composite fibre, comprises the following steps:
(1) preparation homogeneous phase solution, is dissolved in lignocellulose fragment in the boratory dicyandiamide solution of N-ethylpyridine villaumite/1-ethyl-3-methylimidazole, forms homogeneous phase solution;
(2) preparation co-blended spinning solution, by a certain amount of biology enzyme powder, is dissolved in the homogeneous phase solution described in (1) step, forms the heterogeneous Polymer Solution system mixing, and is 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) spinning biology enzyme/lignocellulose composite fibre, adopt wet spinning or electrostatic spinning technique by (3) step spinning solution, be spun into the composite fibre or the nano-composite fiber felt that carry biology enzyme/lignocellulose, and to its carry out rinsing, product is dried, dehumidifies and to obtain.
2. according to the preparation method of a kind of biology enzyme/lignocellulose composite fibre claimed in claim 1, it is characterized in that comprising the following steps:
(1) preparation homogeneous phase solution, is dissolved in lignocellulose fragment in the boratory ionic liquid mixed solvent system of N-ethylpyridine villaumite/1-ethyl-3-methylimidazole, forms homogeneous phase solution;
(2) preparation co-blended spinning solution, by a certain amount of biology enzyme powder, is dissolved in the homogeneous phase solution described in (1) step under room temperature, forms the heterogeneous Polymer Solution system mixing, and is mixed with the co-blended spinning solution mixing;
(3) spinning solution processed, obtains spinning solution by the co-blended spinning solution deaeration described in (2) step, filtration under room temperature;
(4) spinning biology enzyme/lignocellulose composite fibre, under room temperature, adopt wet spinning or electrostatic spinning technique, by (3) step spinning solution, be spun into the composite fibre or the nano-composite fiber felt that carry biology enzyme/lignocellulose, and first carry out after rinsing 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) is controlled N-ethylpyridine villaumite and the boratory quality mol ratio of 1-ethyl-3-methylimidazole is 1.00-7.59; The degree of polymerization of lignocellulose is 600-2000, and lignocellulose fragment solution temperature is 60 ℃-120 ℃, and in homogeneous phase solution, the quality hundred of lignocellulose is than being 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 described biology enzyme be in papain, chymopapain A, chymopapain B, pawpaw PEPB B any one.
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 the middle mass concentration of controlling biology enzyme in co-blended spinning solution of described step (2) is 0.01%-8.33%.
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) wet spinning condition is: the time of 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 reeling, the compacting by drying temperature of fiber is 30
oc-60
oc; The fibre single thread fiber number of spinning is that 2.2dtex-3.2dtex, intensity are 0.9 cN/dtex-2.8cN/dtex.
7. 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) electrostatic spinning condition is: in syringe, spinning solution flow velocity is 0.7-1.5 mL/h, the voltage applying is 12-14 kV, and two interpolar screen needle gages are 14-19 cm; The baking temperature of the nano-composite fiber felt of spinning is 30 ℃-60 ℃, and be 3-5 hour drying time.
8. biology enzyme/lignocellulose composite fibre prepares according to the method described in claim 1 or 2.
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| CN105040136A (en) * | 2015-06-13 | 2015-11-11 | 浪莎针织有限公司 | Cellulose acetate wet spun fiber loaded with medicine for treating local inflammation and pain and preparation method of cellulose acetate wet spun fiber |
| CN111379038A (en) * | 2020-04-23 | 2020-07-07 | 罗莱生活科技股份有限公司 | Skin care fiber and preparation method and application thereof |
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| JP2000226720A (en) * | 1999-02-04 | 2000-08-15 | Kuraray Co Ltd | Cellulose yarn having controlled fibrillation and its production |
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