CN104894695A - Collagen fiber capable of being directly used for spinning and dermal fiber leather prepared by the same - Google Patents
Collagen fiber capable of being directly used for spinning and dermal fiber leather prepared by the same Download PDFInfo
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- CN104894695A CN104894695A CN201510228478.4A CN201510228478A CN104894695A CN 104894695 A CN104894695 A CN 104894695A CN 201510228478 A CN201510228478 A CN 201510228478A CN 104894695 A CN104894695 A CN 104894695A
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Abstract
The invention discloses a collagen fiber capable of being directly used for spinning and dermal fiber leather prepared by the same. The collagen fiber is obtained by utilizing the strong effect of a polar solvent rich in hydroxyl groups and the combination of an ultrasonic treatment mode to achieve dissociation of intermolecular high-crystallized hydrogen bonds on the conditions of great mildness, obtaining raw material loosed in structure, performing drum treatment softening, liquid fiber separation and fiber drying, and then performing treatment on the dried collagen fiber in a single fiber state in combination with electrical impulse of an appropriate strength on the conditions of nitrogen protection. The preparation process is clean and free of pollution, and the manufactured collagen fiber can be directly spun through an existing spinning process without needing graft modification or compounding.
Description
Technical field
The present invention relates to a kind of for weave, can direct spinning collagenous fibres and corium fabric leather prepared therefrom, specifically one can direct spinning collagenous fibres and corium fabric leather prepared therefrom.
Background technology
Along with the development of leather industry, leather processing procedure solid waste discharge amount also increases thereupon, and the pollution problem to environment brought thus, under the route of sustainable development, cleaner production instructs, obtains increasing attention.In solid leather wastes, except a small amount of animal wool, meat, its main component be carry out pruning at the wet blue leather of leather processing procedure, leftover pieces, the leftover bits and pieces when process such as to cut.This type of wet blue leather leftover bits and pieces is mutually interted by corium fabric and collagenous fibres to be interwoven, and collagenous fibres account for 95% ~ 98% of the whole fiber quality of whole corium.
Collagenous fibres molecule is bar-shaped, its composition is I-type collagen, containing three α polypeptide chains, be wound mutually right-handed helix structure, triple helix forms a determining deviation, in longitudinal symmetrical staggered fibrillation, the orderly gathering of triple helix molecule makes collagenous fibres have certain intensity and toughness, and then forms larger fibre bundle.The natural characteristic that collagenous fibres master has such as hygroscopicity, gas permeability, comfortableness etc. exceed cotton, also have strong, wear-resisting, fire-retardant, fungi-proofing, the disconnected heat of the stretching resistance that cotton do not possess, sound-absorbing simultaneously, resist the performances such as wrinkling; Collagenous fibres heat insulation effect is better than eider down, has the gloss as silk, the feel as cashmere; Collagen is described as " bone in bone ", " skin in skin ", it organizes almost identical with human skin tissue, to human skin have 95% similar, exceed the fine fibre of silk in natural fabric and the similar of human skin 85%, easily be attached to skin and hair surface, it has peculiar compatibility to human body; Simultaneously collagenous fibres can spin raw material, fill series of products etc. and also have good bulkiness, resilience, warming good, fire-retardant, sound-absorbing, and free from extraneous odour, without putrefaction go mouldy, and the dramatic benefit such as can to wash.
In traditional leather industry, owing to being subject to the restriction of the factor such as congenital quality, shape, area of animal's leather, the demand of people to high-end leather and fur products cannot be met, in the case, the Synthetic Leather being base cloth with three-dimensional net structure not weaving fabric of superfine fiber is owing to having the intrinsic sucting wet air permeability of natural leather, and exceed natural leather and developed rapidly in chemical resistance, waterproof, anti-mildew etc., superfine fibre also becomes a focus textile raw material of each textile manufacturing enterprise development grade textiles both at home and abroad.As the high-end product of artificial leather synthetic leather industry---superfine fiber chemical leather, its use effectively improves class and the added value of product, but, because this type of synthetic leather is mainly synthesized by chemical fibre, its sanitation performance, still there is larger gap with natural fabric with the affinity etc. of people.
Based on the characteristic of collagenous fibres self, it has many advantages compared to chemical synthesis fibrid, develop leather industry solid waste, the collagenous fibres extracted wherein are effective ways that the problem of environmental pollution solving leather industry also can improve the utilization rate of resource simultaneously.
In prior art, disclose the method extracting collagenous fibres in animal's leather.Such as, CN 102492998 B discloses a kind of method extracting collagenous fibres from tanning leftover, specifically first select block wet blue waste material, adopt dipping by lye wet blue waste material 36-48 hour, by swelling wet blue waste material ultrasonic equipment process 20-30 minute; Then, wet blue waste material is slow transitted through high-voltage water jet device; Then dry, eventually pass further strike and the shredding of carding machine, make thoroughly to produce separation between collagenous fibres, obtain collagenous fibres.CN 103696031 A discloses and a kind ofly prepares the method for collagenous fibres and the application of obtained product and product, and described method comprises step: s1, carry out preliminary treatment to leather material; S5, to carrying out pretreated leather material shredding, made described collagenous fibres.Wherein, for the ease of shredding, and improve the performance of obtained collagenous fibres, at least one in comprising the following steps in pre-treatment step: active bacteria is softened, pickling makes that leather part acid is swollen, organophosphor tanning, alkali swelling, the process of acrylic acid hydrone, wattle extract tanning, stuffing process etc. under low ph condition.
CN102492998 discloses a kind of method extracting fiber from tanning leftover, and it adopts dipping by lye wet blue waste material 36-48 hour, by swelling wet blue waste material ultrasonic equipment process 20-30 minute; Then, wet blue waste material is slow transitted through high-voltage water jet device; Then dry, eventually pass further strike and the shredding of carding machine, make thoroughly to produce separation between collagenous fibres, obtain collagenous fibres.
The mode of the process that prior art is mainly combined by physics, chemistry or physics and chemistry makes collagenous fibres loose in leather, is aided with subsequent treatment and makes it be separated and obtain.Again in conjunction with the mode of physical treatment after employing chemical treatment, as pickling swelling, alkalescence swollen, ferment treatment etc. easily make collagenous fibres that softening or overgenerous chemical environment occurs under chemical environment to make tropocollagen molecule destructurized, expose combinative end group or be broken into Small molecular group, produce fibre debris, the active force produced through follow-up physical treatment is again larger, cause fibrillation impaired, decreasing can conjugated group, make when the production for the preparation of yarn and fabric, easy generation adhesion is not enough, cause formed leather tension force uneven, easy scratch, the defects such as fracture, be not suitable for processing and the production of high-end real leather products, the fibre debris produced also runs off along with process, causes the waste of resource, improves the production cost of target product.
Summary of the invention
The object of this invention is to provide a kind of can the preparation method of direct spinning collagenous fibres, the method utilizes the polar solvent being rich in hydroxyl to pretend use, in conjunction with the mode of ultrasonic process, dissociating of intermolecular high crystallization hydrogen bond is realized under condition as mild as a dove, obtain loosely organized raw material, ease back through rotary drum process, liquid solution is fine, fiber is dried, again by the collagenous fibres of filament state after drying under nitrogen protection condition in conjunction with the Electric Pulse Treatment of suitable intensity, so that fine fiber surface roughness can be increased, increase its binding ability in subsequent handling, fungistatic effect, preparation process cleanliness without any pollution, obtained collagenous fibres are without the need to can directly adopt existing spinning technique to carry out spinning through graft modification or compound, the collagenous fibres adopting the method to prepare carry out spinning, are woven into Ji Bu, the corium fabric leather that reprocessing is formed has that tensile strength is high, wear-resisting, soft, moisture absorption, oil suction, easily contaminate, advantage that fire resistance is good, be particularly suitable for the production of high-end leather and fur products.
Another object of the present invention is to provide a kind of method utilizing above-mentioned preparation method to extract the collagenous fibres obtained to prepare corium fabric leather.
First object of the present invention is achieved through the following technical solutions: a kind of can the preparation method of direct spinning collagenous fibres, be following steps:
(1) shear: take wet blue leather as raw material, be cut into the size of production or equipment requirement with leather cutter;
(2) ultrasonic preliminary treatment: the pretreatment fluid of the polar solvent of hydroxyl is rich in preparation, the consumption of pretreatment fluid is 6-25 times of wet blue leather weight, pH is regulated to be 7 ~ 7.5, be warming up to 40 ~ 50 DEG C, be placed in one the wet blue leather cut immersion 12 ~ 24 hours, then pretreatment fluid is warming up to 50 ~ 60 DEG C, pH is regulated to be 7.5 to 8, soak 1 ~ 2 hour again, under Current Temperatures, carry out ultrasonic low frequency vibrate in short-term, the Ultrasonic Conditions adopted is: frequency 20 ~ 50kHz, power 200 ~ 600W, ultrasonic time 10 ~ 20 minutes; Wherein, the pretreatment fluid being rich in the polar solvent of hydroxyl described in is according to volume ratio 1:(1 ~ 5 by the alcoholic solution of the alkaline solution of mass concentration 2 ~ 10% and mass concentration 45 ~ 75%) mix obtained;
(3) rotary drum process: ultrasonic process terminates, elimination pretreatment fluid, pretreated wet blue leather is adopted rotary drum treatment process, first in aqueous environment, rotary drum is rotated, rotary drum rotating speed is 8-15 rev/min, time is 5 minutes, then rotary drum is stopped, discharge liquid, and then water is added in rotary drum, and in aqueous environment, add softener amino silicon oil emulsion or ternary polymerization silicone oil emulsion gradually, after slow rotation rotary drum mixing fully, then rotate rotary drum again and carry out the process that eases back, rotary drum rotating speed is 6-10 rev/min, temperature is 25 DEG C, time is 3-4 hour,
(4) liquid solution fibre, fiber are dried: the wet blue leather eased back through rotary drum process, preliminary shredding is proceeded to liquid fiber uncoiling machine, the centrifugal force produced by hydraulic mixing, by collagenous fibres with textile fabric form out; Then by dryer, the collagenous fibres separated from liquid fiber uncoiling machine are dried in baking indoor, the mode that furnace drying method adopts exhausting and air intake to combine, exhausting is adopted to be carried as dried indoor by air inlet mode again by drying after indoor humid air extracts drying out, circulation like this is dried, until the moisture 25 ~ 35% of fiber, adopt bake out temperature to be 70 ~ 80 DEG C;
(5) shredding removal of impurities, combing: adopt opening to carry out shredding the fiber after drying, opening process is, opening roller diameter be Φ 380mm, rotating speed carries out shredding process under being the parameter of 600rpm, and eliminates the impurity beyond fiber, obtains bunchy collagenous fibres; Again by carding machine, the collagenous fibres of bunchy are carded to the collagenous fibres of filament state, the design parameter on carding machine is, temperature is 27 DEG C, humidity is 70%-75%, go out net spee is 3.5m/min;
(6) Fiber strength: collagenous fibres step (5) obtained are placed in impulse electric field and carry out surface treatment under nitrogen protection condition, and treatment conditions are: pulse frequency 20 ~ 30Hz, electric-field intensity are 20kV/cm, processing time 1 ~ 10s.
In technique scheme, aqueous slkali can be one or both the combination in sodium hydroxide solution, sodium bicarbonate solution; Described alcoholic solution is the combination of one or more in ethanolic solution, isopropyl alcohol, n-butanol, propylene glycol, polyglycol solution.
The consumption of pretreatment fluid is can submergence is pending completely wet blue leather raw material be as the criterion.The pH value of preferred pretreatment fluid is 7.2 ~ 7.6.
In the transport of wet blue leather raw material and slicing processes, wet blue leather loses portion of water, need to reuptake moisture, therefore, before carrying out ultrasonic process, also can first wet blue leather raw material to be immersed in pond 2 ~ 5 minutes, oven dry to moisture content 60 ~ 80% carries out ultrasonic preliminary treatment again, the method both can wash away impurity, the moisture of raw material can also be adjusted, after being conducive to fibrous absorbent, when being conducive to follow-up ultrasonic process, pretreatment fluid produces good osmosis by concentration difference, enters into the intermolecular dissociation to intermolecular crystal type hydrogen bond better.
With the operating environment of rotary drum for aqueous phase, be convenient to add softener, make wet blue leather accelerate to ease back, by the mechanism of rotary drum, wet blue leather obtains preliminary shredding; In rotary drum processing procedure, the pretreatment fluid that fibrous inside is residual can also be cemented out by modes of action such as cleaning, difference in height, concentration differences simultaneously, avoid the pretreatment fluid remained to impact fibre structure, thus affect subsequent handling and product quality; Described softener can adopt as softeners such as amino silicon oil emulsion, ternary polymerization silicone oil emulsions, be combined with leather fiber by the amino in softener, hydroxyl, polyether group, the molecular layer that Si-O-Si terminates can be formed at fiber surface, produce soft, smooth feel, and ability selects the softener of different activities group to process as required, obtain leather fiber that is hydrophilic or hydrophobic effect.
Step (4) is described when being dried by fiber, dryer can adopt Steam Heating, and compressor flow can adopt 15000 ~ 20000m3/h, collects the collagenous fibres taken away by bleeding to be back to production, particulate collagenous fibres dust enters dust collecting system, takes out in paper mill.
For ease of combing, fiber requirements has certain degree of opening, fiber after oven dry normally presents is entangled with into large bulk, fritter can be become by shredding program and then become fiber bundle-like, then carding machine is passed through, the collagenous fibres of bunchy are carded to filament state, form the fiber web of one fixed width, certain mass area ratio.During described removal of impurities, adopt dust collecting system to collect fiber grain, take out in paper mill, the collagenous fibres obtained after removal of impurities can mix in proportion according to need of production classification or the collagenous fibres that length, fineness etc. be there are differences large percentage makes it homogenising.
Adopt collagenous fibres length 5 ~ 50mm that technique scheme obtains, fineness 0.5 ~ 3D.
Another object of the present invention is achieved through the following technical solutions: a kind of corium fabric leather, it is the collagenous fibres preparation of the be directly used in spinning adopting the present invention's first technical scheme to obtain, during preparation, the collagenous fibres preparation that first can be directly used in spinning adopts spinning process spun yarn, woven base fabric, then by base cloth through dyeing, dry, draw soft, flour milling, Final finishing to obtain; Staining procedure is in conjunction with ultrasonic wave process when carrying out for described dyeing process, and the ultrasonic wave treatment conditions adopted are as follows: frequency 20 ~ 50kHz, power 200 ~ 600W, ultrasonic time 10 ~ 20 minutes; Described drying carries out micro-wave vacuum at 30 ~ 60 DEG C.
In above-mentioned technical scheme, described spinning process can be according to the different size of obtained collagenous fibres and the different requirements of producing yarn, select to adopt the spinning process be applicable to, as traditional handicrafts such as ring spinning, air-jet spinning, friction spun yarns, or new spinning process, as new technologies such as empty open-end spinning, dry method spinning.Described afterfinish method also can adopt synthetic leather rear section method for sorting to carry out.
Adopt technique scheme, when dyeing, collagenous fibres base cloth through dyestuff scrim surfaces absorption, to base cloth internal layer diffusion, set on base cloth three phases, collagenous fibres generation non-locating can be made to adsorb by adopting ultrasonic wave, increase dyeing affinity, increase colorant dissolubility, make fiber surface that similar etching effect occur; The dye granule of the phenomenons such as ultrasonic wave process can also make easily to assemble, sedimentation resolves into uniform dispersion, improves the diffusion of dyestuff, seepage velocity; Ultrasonic wave process also make dissolving by degasification or be trapped in basic intertwined point, fiber capillary and gap location gas molecule expulsion in solution, and get rid of thereupon, stickiness block layer can be made thinning by diffusion, be conducive to accelerating dye solution and be diffused into fibrous inside.
The dry run of technique scheme, by the radiant heating in vacuum effect of microwave, reaches painting cloth solid form, the object of the inner chemical materials of fixed base cloth.Painting cloth after microwave drying easily produces the phenomenons such as plate is hard, warpage, and by drawing soft stretching, extension, make fiber loose soft, high resilience, the smooth softness of painting cloth of acquisition, without curling, area slightly increases.
After drawing the painting cloth of soft rear acquisition to stretch, can expose the nibs on surface, can eliminate such flaw by flour milling, auxiliary uniform thickness, improves the physical property of painting cloth, prepares for covering with paint, lacquer, colour wash, etc.
Auxiliary agent is added by adopting at finishing process, as face finish, surface conditioning agent, anti-anaphylaxis agent, mould inhibitor, anti-fouling agent, deodorant, fire retardant etc., increase the additional properties of corium fabric leather product, such as increase its health care, as comprised hypo-allergenic property, anion function, hygienic function comprises antibacterial and deodouring, mildew-resistant, antifouling etc., and safeguard function comprises antiultraviolet, antistatic, fire-retardant etc.
The corium fabric leather that employing technique scheme prepares is for making top grade leather fabric leather goods, as high-grade leatherware case and bag, high-grade clothing, high-grade leather packaging material etc., or have tensile strength, anti-wear performance, softness, moisture pick-up properties, oil preventing performance, resist printing performance, fire resistance etc. to require high corium fabric leather product to weaving material, as the Work Clothes of field tent, anorak, warm-up, field training clothes, turnout gear, combustible and explosive area dress.
The preparation method of collagenous fibres of the present invention is by adopting the cooperation process in conjunction with key technology techniques such as the Electric Pulse Treatment of suitable intensity under polar solvent, ultrasonic preliminary treatment, nitrogen protection condition, as follows relative to the beneficial effect of prior art:
(1) by adopting the macromolecular intermolecular hydrogen bonding of polar solvent resolution, embed Small molecular polyphenol, new molecular association body is compounded to form again by hydrogen bond, what this mode can make full use of the polar solvent being rich in hydroxyl pretends use, under condition as mild as a dove, realize dissociating high crystallization hydrogen bond, be a kind of green chemistry process route; Simultaneously by the change of two stage different pH value, can more effective performance be rich in the polar solvent of hydroxyl pretend use;
(2) by step by step rotary drum softening process, make can supple-settlement Be very effective improve;
(3) ultrasonic process preliminary treatment produces cavitation, and make molecular structure loose, the fracture and the Small molecular polyphenol that are conducive to later stage intermolecular hydrogen bonding enter in the middle of molecular structure, form stable molecular association body; Ultrasonic process also accelerates the fractionation of polar solvent to macromolecular intermolecular hydrogen bonding, and Reaction time shorten, enhances productivity;
(4) under nitrogen protection condition in conjunction with the Electric Pulse Treatment of suitable intensity, fine fiber surface roughness can be increased, increase its interfibrous adhesion in follow-up spinning process, formed and there is the Ji Bu of sufficient intensity, to improve the mar proof of corium fabric leather finished product, scratch resistance and binding strength; Electric field pulse process can also make the moisture being trapped in fibrocyte inside discharge after fibrocyte perforate membrane, also has the effect of sterilization simultaneously, plays a protective role to the collagenous fibres of preparation, reduce the antibacterial cost of real leather products.
Wet blue leather of the present invention refer to animal hides leather through deoiling, degrease, depilation, after chrome tanning process containing certain moisture, present blue wet pelt leather, described animal's leather can be conventional animal, as horse, ox, sheep, dog, pig, rabbit, crocodile, snake, deer, donkey, mule, camel, kangaroo etc. can be used for the leather of the animal as leather raw materials for production, the above-mentioned two kinds of technical schemes of the present invention are not only applicable to wet blue leather leftover bits and pieces, the animal's leather of tanning is also suitable for, there is very strong practicality and apply meaning.
The present invention is different from and main adopts needle point method to make the method for non-weaving cloth fibrillation making synthetic leather base as reinforcing means, the mixed fibre that to account for 40 ~ 60% with extraction fiber, also be different from after leftover bits and pieces is dissolved and carry out spinning, and then carry out the method for rear road processing.Corium fabric leather of the present invention from wet blue leather, extracts the collagenous fibres that can be directly used in spinning be prepared, the extraction process feature of environmental protection of its collagenous fibres is strong, the collagenous fibres obtained have very strong adhesion and good physical characteristic, obtained corium fabric leather can realize industrialized standard and produce by the standard area often opening leather 1.5m × 1.5m, well overcome the various defects such as animal's leather tension force is irregular, easy scratch, the preparation of very suitable high-end real leather products.
Accompanying drawing explanation
Fig. 1 is after collagenous fibres Direct Spinning resultant yarn of the present invention, then with the configuration of surface (atomic force microscope images) of the fabric of the weaving yarns be spun into one-tenth, wherein Fig. 1 a is graphics, and Fig. 1 b is phase diagram.
Detailed description of the invention
Be described in further details the present invention below by embodiment, these embodiments are only used for the present invention is described, do not limit the scope of the invention.
Embodiment 1 adopts following steps to prepare a kind of collagenous fibres being directly used in spinning:
(1) shear: take wet blue leather as raw material, be cut into the size of production or equipment requirement with leather cutter;
(2) ultrasonic preliminary treatment: prepare pretreatment fluid, pH is regulated to be 7 ~ 7.5, heat up 40 ~ 50 DEG C, the wet blue leather cut is immersed in completely pretreatment fluid and soaks 12-24 hour, then pretreatment fluid is warming up to 50-60 DEG C, pH is regulated to be 7.5 to 8, soak 1-2 hour again, under Current Temperatures, carry out ultrasonic low frequency vibrate in short-term, the Ultrasonic Conditions adopted is: frequency 20-50kHz, power 200 ~ 600W, ultrasonic time 10-20 minute; Pretreatment fluid is according to volume ratio 1:(1 ~ 5 by the sodium hydroxide solution of mass concentration 2-10% and the butanol solution of mass concentration 45-75%) mix obtained;
(3) rotary drum process: ultrasonic process terminates, elimination pretreatment fluid, pretreated wet blue leather is adopted rotary drum treatment process, first in aqueous environment, rotary drum is rotated, rotary drum rotating speed is 8-15 rev/min, time is 5 minutes, then stop rotary drum, discharge liquid, and then add water in rotary drum, and in aqueous environment, add softener ternary polymerization silicone oil emulsion gradually, after slow rotation rotary drum mixing fully, more then rotation rotary drum carries out the process that eases back, and rotary drum rotating speed is 6-10 rev/min, temperature is 25 DEG C, and the time is 3-4 hour;
(4) liquid solution fibre, fiber are dried: the wet blue leather eased back through rotary drum process, preliminary shredding is proceeded to liquid fiber uncoiling machine, the centrifugal force produced by hydraulic mixing, by collagenous fibres with textile fabric form out; Then by dryer, the collagenous fibres separated from liquid fiber uncoiling machine are dried in baking indoor, the mode that furnace drying method adopts exhausting and air intake to combine, exhausting is adopted to be carried as dried indoor by air inlet mode again by drying after indoor humid air extracts drying out, circulation like this is dried, until the moisture 25 ~ 35% of fiber, adopt bake out temperature to be 70 ~ 80 DEG C;
(5) shredding removal of impurities, combing: adopt opening to carry out shredding the fiber after drying, opening process is, opening roller diameter be Φ 380mm, rotating speed carries out shredding process under being the parameter of 600rpm, and eliminates the impurity beyond fiber, obtains bunchy collagenous fibres; Again by carding machine, the collagenous fibres of bunchy are carded to the collagenous fibres of filament state, the design parameter on carding machine is, temperature is 27 DEG C, humidity is 70%-75%, go out net spee is 3.5m/min;
(6) Fiber strength: collagenous fibres step (5) obtained are placed in impulse electric field and carry out surface treatment under nitrogen protection condition, and treatment conditions are: pulse frequency 20Hz, electric-field intensity are 20kV/cm, processing time 5s.
Embodiment 2 adopts following steps to prepare a kind of collagenous fibres being directly used in spinning:
(1) shear: take wet blue leather as raw material, be cut into the size of production or equipment requirement with leather cutter;
(2) ultrasonic preliminary treatment: the polar solvent pretreatment fluid of hydroxyl is rich in preparation, pH is regulated to be 7, be warming up to 45 DEG C, the wet blue leather cut be immersed in pretreatment fluid completely and soak 24 hours, then pretreatment fluid is warming up to 50 DEG C, pH is regulated to be 7.5 to 8, soak 2 hours again, under Current Temperatures, carry out ultrasonic low frequency vibrate in short-term, the Ultrasonic Conditions adopted is: frequency 20kHz, power 200W, ultrasonic time 20 minutes; Pretreatment fluid mixes obtained by the sodium hydroxide solution of mass concentration 2% according to volume ratio 1:1 with the polyglycol solution of mass concentration 75%;
(3) rotary drum process: ultrasonic process terminates, elimination pretreatment fluid, pretreated wet blue leather is adopted rotary drum treatment process, first in aqueous environment, rotary drum is rotated, rotary drum rotating speed is 15 revs/min, time is 5 minutes, then stop rotary drum, discharge liquid, and then add water in rotary drum, and in aqueous environment, add softener amino silicon oil emulsion gradually, after slow rotation rotary drum mixing fully, more then rotation rotary drum carries out the process that eases back, and rotary drum rotating speed is 10 revs/min, temperature is 25 DEG C, and the time is 3 hours;
(4) liquid solution fibre, fiber are dried: liquid solution is fine, fiber is dried: the wet blue leather eased back through rotary drum process, preliminary shredding is proceeded to liquid fiber uncoiling machine, the centrifugal force produced by hydraulic mixing, by collagenous fibres with textile fabric form out; Then by dryer, the collagenous fibres separated from liquid fiber uncoiling machine are dried in baking indoor, the mode that furnace drying method adopts exhausting and air intake to combine, exhausting is adopted to be carried as dried indoor by air inlet mode again by drying after indoor humid air extracts drying out, circulation like this is dried, until the moisture 30% of fiber, adopt bake out temperature to be 75 DEG C;
(5) adopt opening to carry out shredding the fiber after drying, opening process is, opening roller diameter be Φ 380mm, rotating speed carries out shredding process under being the parameter of 600rpm, and eliminates the impurity beyond fiber, obtains bunchy collagenous fibres; Again by carding machine, the collagenous fibres of bunchy are carded to the collagenous fibres of filament state, the design parameter on carding machine is, temperature is 27 DEG C, humidity is 75%, go out net spee is 3.5m/min;
(6) Fiber strength: collagenous fibres step (5) obtained are placed in impulse electric field and carry out surface treatment under nitrogen protection condition, and treatment conditions are: pulse frequency 25Hz, electric-field intensity are 20kV/cm, processing time 10s.
Embodiment 3 adopts following steps to prepare a kind of collagenous fibres being directly used in spinning:
(1) shear: take wet blue leather as raw material, be cut into production or the size of equipment requirement with leather cutter, wet blue leather raw material to be immersed in pond 2 ~ 5 minutes, dry to moisture content 60 ~ 80%;
(2) ultrasonic preliminary treatment: prepare pretreatment fluid, pH is regulated to be 7, be warming up to 50 DEG C, wet blue leather be immersed in completely pretreatment fluid and soak 12 hours, then pretreatment fluid is warming up to 55 DEG C, pH is regulated to be 7.5, soak 1.5 hours again, under Current Temperatures, carry out ultrasonic low frequency vibrate in short-term, the Ultrasonic Conditions adopted is: frequency 40kHz, power 600W, ultrasonic time 10 minutes; Pretreatment fluid according to volume ratio 1:5 mixes obtained with the isopropyl alcohol of mass concentration 45% with mixed with propylene glycol solution (isopropyl alcohol and propylene glycol volume ratio are 2:3) by the sodium hydroxide solution of mass concentration 10%;
(3) rotary drum process: ultrasonic process terminates, elimination pretreatment fluid, pretreated wet blue leather is adopted rotary drum treatment process, first in aqueous environment, rotary drum is rotated, rotary drum rotating speed is 8 revs/min, time is 5 minutes, then stop rotary drum, discharge liquid, and then add water in rotary drum, and in aqueous environment, add softener amino silicon oil emulsion gradually, after slow rotation rotary drum mixing fully, more then rotation rotary drum carries out the process that eases back, and rotary drum rotating speed is 8 revs/min, temperature is 25 DEG C, and the time is 4 hours;
(4) liquid solution fibre, fiber are dried: liquid solution is fine, fiber is dried: the wet blue leather eased back through rotary drum process, preliminary shredding is proceeded to liquid fiber uncoiling machine, the centrifugal force produced by hydraulic mixing, by collagenous fibres with textile fabric form out; Then by dryer, the collagenous fibres separated from liquid fiber uncoiling machine are dried in baking indoor, the mode that furnace drying method adopts exhausting and air intake to combine, exhausting is adopted to be carried as dried indoor by air inlet mode again by drying after indoor humid air extracts drying out, circulation like this is dried, until the moisture 35% of fiber, adopt bake out temperature to be 70 DEG C;
(5) adopt opening to carry out shredding the fiber after drying, opening process is, opening roller diameter be Φ 380mm, rotating speed carries out shredding process under being the parameter of 600rpm, and eliminates the impurity beyond fiber, obtains bunchy collagenous fibres; Again by carding machine, the collagenous fibres of bunchy are carded to the collagenous fibres of filament state, the design parameter on carding machine is, temperature is 27 DEG C, humidity is 70%, go out net spee is 3.5m/min;
(6) Fiber strength: collagenous fibres step (5) obtained are placed in impulse electric field and carry out surface treatment under nitrogen protection condition, and treatment conditions are: pulse frequency 30Hz, electric-field intensity are 20kV/cm, processing time 3s.
Embodiment 4 adopts following steps to prepare a kind of collagenous fibres being directly used in spinning:
(1) shear: take wet blue leather as raw material, be cut into the size of production or equipment requirement with leather cutter;
(2) ultrasonic preliminary treatment: prepare pretreatment fluid, pH is regulated to be 7.5, heat up 40 DEG C, the wet blue leather cut is immersed in pretreatment fluid completely and soaks 20 hours, then pretreatment fluid is warming up to 60 DEG C, pH is regulated to be 7.5, soak 1 hour again, under Current Temperatures, carry out ultrasonic low frequency vibrate in short-term, the Ultrasonic Conditions adopted is: frequency 50kHz, power 400W, ultrasonic time 15 minutes; Pretreatment fluid mixes obtained by the sodium hydroxide solution of mass concentration 5% according to volume ratio 1:3 with the polyglycol solution of mass concentration 50%;
(3) rotary drum process: ultrasonic process terminates, elimination pretreatment fluid, pretreated wet blue leather is adopted rotary drum treatment process, first in aqueous environment, rotary drum is rotated, rotary drum rotating speed is 10 revs/min, time is 5 minutes, then stop rotary drum, discharge liquid, and then add water in rotary drum, and in aqueous environment, add softener ternary polymerization silicone oil emulsion gradually, after slow rotation rotary drum mixing fully, more then rotation rotary drum carries out the process that eases back, and rotary drum rotating speed is 10 revs/min, temperature is 25 DEG C, and the time is 3.5 hours;
(4) liquid solution fibre, fiber are dried: the wet blue leather eased back through rotary drum process, preliminary shredding is proceeded to liquid fiber uncoiling machine, the centrifugal force produced by hydraulic mixing, by collagenous fibres with textile fabric form out; Then by dryer, the collagenous fibres separated from liquid fiber uncoiling machine are dried in baking indoor, the mode that furnace drying method adopts exhausting and air intake to combine, exhausting is adopted to be carried as dried indoor by air inlet mode again by drying after indoor humid air extracts drying out, circulation like this is dried, until the moisture 25% of fiber, adopt bake out temperature to be 80 DEG C;
(5) shredding removal of impurities, combing: adopt opening to carry out shredding the fiber after drying, opening process is, opening roller diameter be Φ 380mm, rotating speed carries out shredding process under being the parameter of 600rpm, and eliminates the impurity beyond fiber, obtains bunchy collagenous fibres; Again by carding machine, the collagenous fibres of bunchy are carded to the collagenous fibres of filament state, the design parameter on carding machine is, temperature is 27 DEG C, humidity is 75%, go out net spee is 3.5m/min;
(6) Fiber strength: collagenous fibres step (5) obtained are placed in impulse electric field and carry out surface treatment under nitrogen protection condition, and treatment conditions are: pulse frequency 20Hz, electric-field intensity are 20kV/cm, processing time 5s.
The collagenous fibres preparation of the be directly used in spinning that embodiment 5 Example 1 prepares prepares corium fabric leather as follows: the collagenous fibres preparation of the be directly used in spinning that Example 1 prepares adopts RING SPINNING spinning process spun yarn, woven base fabric, again base cloth is passed through dyeing, at 50 DEG C, carry out micro-wave vacuum do, staking machine draws soft, flour milling, add finishing agent, mould inhibitor, fire retardant carries out Final finishing and obtains, dyeing process when carrying out staining procedure in conjunction with ultrasonic wave process, the ultrasonic wave treatment conditions adopted are as follows: frequency 30kHz, power 500W, ultrasonic time 15 minutes.
Claims (7)
1. can the preparation methods of direct spinning collagenous fibres, it is characterized in that: adopt following steps:
(1) shear: take wet blue leather as raw material, be cut into the size of production or equipment requirement with leather cutter;
(2) ultrasonic preliminary treatment: the pretreatment fluid of the polar solvent of hydroxyl is rich in preparation, the consumption of pretreatment fluid is 6-25 times of wet blue leather weight, pH is regulated to be 7 ~ 7.5, be warming up to 40 ~ 50 DEG C, be placed in one the wet blue leather cut immersion 12 ~ 24 hours, then pretreatment fluid is warming up to 50 ~ 60 DEG C, pH is regulated to be 7.5 to 8, soak 1 ~ 2 hour again, under Current Temperatures, carry out ultrasonic low frequency vibrate in short-term, the Ultrasonic Conditions adopted is: frequency 20 ~ 50kHz, power 200 ~ 600W, ultrasonic time 10 ~ 20 minutes; Wherein, the described pretreatment fluid being rich in the polar solvent of hydroxyl is according to volume ratio 1:(1 ~ 5 by the alcoholic solution of the alkaline solution of mass concentration 2 ~ 10% and mass concentration 45 ~ 75%) mix obtained, described aqueous slkali is one or both the combination in sodium hydroxide solution, sodium bicarbonate solution, and described alcoholic solution is the combination of one or more in ethanolic solution, isopropyl alcohol, n-butanol, propylene glycol, polyglycol solution;
(3) rotary drum process: ultrasonic process terminates, elimination pretreatment fluid, pretreated wet blue leather is adopted rotary drum treatment process, first in aqueous environment, rotary drum is rotated, rotary drum rotating speed is 8-15 rev/min, time is 5 minutes, then rotary drum is stopped, discharge liquid, and then water is added in rotary drum, and in aqueous environment, add softener amino silicon oil emulsion or ternary polymerization silicone oil emulsion gradually, after slow rotation rotary drum mixing fully, then rotate rotary drum again and carry out the process that eases back, rotary drum rotating speed is 6-10 rev/min, temperature is 25 DEG C, time is 3-4 hour,
(4) liquid solution fibre, fiber are dried: the wet blue leather eased back through rotary drum process, preliminary shredding is proceeded to liquid fiber uncoiling machine, the centrifugal force produced by hydraulic mixing, by collagenous fibres with textile fabric form out; Then by dryer, the collagenous fibres separated from liquid fiber uncoiling machine are dried in baking indoor, the mode that furnace drying method adopts exhausting and air intake to combine, exhausting is adopted to be carried as dried indoor by air inlet mode again by drying after indoor humid air extracts drying out, circulation like this is dried, until the moisture 25 ~ 35% of fiber, adopt bake out temperature to be 70 ~ 80 DEG C;
(5) shredding removal of impurities, combing: adopt opening to carry out shredding the fiber after drying, opening process is, opening roller diameter be Φ 380mm, rotating speed carries out shredding process under being the parameter of 600rpm, and eliminates the impurity beyond fiber, obtains bunchy collagenous fibres; Again by carding machine, the collagenous fibres of bunchy are carded to the collagenous fibres of filament state, the design parameter on carding machine is, temperature is 27 DEG C, humidity is 70%-75%, go out net spee is 3.5m/min;
(6) Fiber strength: collagenous fibres step (5) obtained are placed in impulse electric field and carry out surface treatment under nitrogen protection condition; obtained can direct spinning collagenous fibres; described surface treatment condition is: pulse frequency 20 ~ 30Hz, electric-field intensity are 20kV/cm, processing time 1 ~ 10s.
2. preparation method according to claim 1, is characterized in that: before carrying out ultrasonic process, first to be immersed by wet blue leather raw material in pond 2 ~ 5 minutes, dries to moisture content 60 ~ 80% and carries out ultrasonic preliminary treatment again.
3. preparation method according to claim 1, is characterized in that: the consumption of described pretreatment fluid is soaking completely
Pending wet blue leather raw material is not had to be as the criterion.
4. preparation method according to claim 1, is characterized in that: step (4) is described when being dried by fiber, and dryer adopts Steam Heating, compressor flow 15000 ~ 20000m3/h.
5. preparation method according to claim 1, is characterized in that: what adopt this preparation method to obtain can direct spinning collagenous fibres length 5 ~ 50mm, fineness 0.5 ~ 3D.
6. preparation method according to claim 1, is characterized in that: the pH value of described pretreatment fluid is 7.2 ~ 7.6.
7. a corium fabric leather, it is characterized in that: the collagenous fibres preparation of the be directly used in spinning adopting the preparation method of claim 1 to obtain, during preparation, the collagenous fibres preparation that first can be directly used in spinning adopts spinning process spun yarn, woven base fabric, then by base cloth through dyeing, dry, draw soft, flour milling, Final finishing to obtain; Staining procedure is in conjunction with ultrasonic wave process when carrying out for described dyeing process, and the ultrasonic wave treatment conditions adopted are as follows: frequency 20 ~ 50kHz, power 200 ~ 600W, ultrasonic time 10 ~ 20 minutes; Described drying carries out micro-wave vacuum at 30 ~ 60 DEG C.
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| CN107059142A (en) * | 2017-04-01 | 2017-08-18 | 顾勇杰 | A kind of overlength cattle-hide collagen fibers and its preparation method and application |
| CN107059142B (en) * | 2017-04-01 | 2018-02-13 | 顾勇杰 | A kind of overlength cattle-hide collagen fibers and its preparation method and application |
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| CN107237177A (en) * | 2017-07-03 | 2017-10-10 | 徐琦 | Multifunctional fabric prepared based on collagen fabric fabric and preparation method thereof |
| CN107326688A (en) * | 2017-07-03 | 2017-11-07 | 徐琦 | The method for going back raw hide is prepared based on solvent-free film-forming process incorporating collagen azelon fabric |
| CN107366163A (en) * | 2017-07-03 | 2017-11-21 | 徐琦 | The method for going back raw hide is prepared based on collagen fabric fabric combination flocking technique and solventfree resin technique |
| WO2019007442A3 (en) * | 2017-07-03 | 2019-02-07 | 徐琦 | Collagen fibre grey cloth and hydroentanglement process-based method for preparing reconstituted leather |
| CN108251905A (en) * | 2018-01-19 | 2018-07-06 | 嘉兴奥克兰特种牛皮科技有限公司 | The preparation method of cattle-hide collagen fibers and its cattle-hide collagen fibers obtained and application |
| WO2020239113A1 (en) * | 2019-05-27 | 2020-12-03 | 广东五源新材料科技集团有限公司 | Animal leather fiber bundle having nanoscale branches, yarn, core-spun yarn and product |
| CN114427134A (en) * | 2019-05-27 | 2022-05-03 | 广东五源新材料科技集团有限公司 | Animal leather fiber bundle with nanoscale branches, yarn, core-spun yarn and product |
| US11613828B2 (en) | 2019-05-27 | 2023-03-28 | Guangdong Wuyuan New Material Technology Group Co., Ltd. | Animal leather fiber bundles, yarns, core-spun yarns and products with nanoscale branches |
| CN114427134B (en) * | 2019-05-27 | 2023-10-31 | 广东五源新材料科技集团有限公司 | Animal leather fiber bundle, yarn, core spun yarn and product with nanoscale branches |
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