CN104894695B - Can direct spinning with preparation method and the corium fabric leather of collagenous fibres - Google Patents
Can direct spinning with preparation method and the corium fabric leather of collagenous fibres Download PDFInfo
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/66—Disintegrating fibre-containing textile articles to obtain fibres for re-use
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- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a kind of can direct spinning collagenous fibres preparation method and the corium fabric leather of being prepared by these collagenous fibres. Collagenous fibres of the present invention are to utilize the polar solvent that is rich in hydroxyl to pretend use; in conjunction with the mode of ultrasonic processing; under condition as mild as a dove, realize dissociating of intermolecular high crystallization hydrogen bond; obtain loosely organized raw material; through rotary drum processing ease back, liquid solution fibre, fiber dry; again the collagenous fibres of the ultimate fibre state after drying are processed and obtained in conjunction with the electric pulse of suitable intensity under nitrogen protection condition; preparation process cleanliness without any pollution, the collagenous fibres that make are without through graft modification or compoundly can directly adopt existing spinning technique to carry out spinning.
Description
Technical field
The present invention relates to a kind of for weave use, can direct spinning with collagenous fibres and corium fabric leather prepared therefrom, specifically one can be for 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, brought thus to the pollution problem of environment under the route of sustainable development, cleaner production instructs, obtained increasing attention. In solid leather wastes, except a small amount of animal wool, meat, its main component is leftover pieces, the leftover bits and pieces while processing such as to prune, cut at the wet blue leather of leather processing procedure. This type of wet blue leather leftover bits and pieces is to be that collagenous fibres mutually intert and are interwoven by corium fabric, and collagenous fibres have accounted for 95%～98% of the whole fiber qualities of whole corium.
Collagenous fibres molecule is bar-shaped, its composition is type i collagen albumen, contain three α polypeptide chains, be wound mutually right-handed helix structure, triple helix forms a determining deviation, is the staggered fibrillation of longitudinal symmetry, 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 is as hygroscopicity, gas permeability, comfortableness etc. exceed cotton, also has strong, wear-resisting, fire-retardant, fungi-proofing, the disconnected heat of stretching resistance, sound-absorbing that cotton do not possess simultaneously, resists 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, the fine fibre that exceedes in natural fiber silk is similar to 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 are gone mouldy, and the dramatic benefit such as can wash.
In traditional leather industry, owing to being subject to the restriction of the factors such as the congenital quality, shape, area of animal's leather, cannot meet the demand of people to high-end leather and fur products, in the case, the Synthetic Leather that is 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 at aspects such as chemical resistance, waterproof, mildew-resistant sex change, superfine fibre also becomes a focus textile raw material of each weaving manufacturing enterprise exploitation grade textiles both at home and abroad. As the high-end product of artificial leather synthetic leather industry---superfine fiber chemical leather, its use has effectively improved class and the added value of product, but, because this type of synthetic leather is mainly to be synthesized by chemical fibre, its sanitation performance, still there is larger gap with natural fiber with people's affinity etc.
Based on the characteristic of collagenous fibres self, it has many advantages compared to chemical synthesis fiber, develop leather industry solid waste, extraction collagenous fibres are wherein effective ways that the problem of environmental pollution of solution leather industry also can improve the utilization rate of resource simultaneously.
In prior art, the method for extracting collagenous fibres in animal's leather is disclosed. For example, CN102492998B discloses a kind of method of 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, swelling wet blue waste material is processed to 20-30 minute with ultrasonic equipment; Then, wet blue waste material is slowly passed through to high-voltage water jet device; Then dry, finally by further strike and the shredding of crossing carding machine, make thoroughly to produce and separate between collagenous fibres, obtain collagenous fibres. CN103696031A discloses a kind of application of preparing the method for collagenous fibres and the product making and product, and described method comprises step: s1, leather material is carried out to pretreatment; S5, to carrying out pretreated leather material shredding, make described collagenous fibres. Wherein, for the ease of shredding, and improve the performance of the collagenous fibres that make, at least one in comprising the following steps in pre-treatment step: active bacterium is softening, pickling makes that leather part acid is swollen, alkali swelling under organophosphor tanning, low ph condition, the processing of acrylic acid hydrone, wattle extract tanning, stuffing processing etc.
CN102492998 discloses a kind of method of extracting fiber from tanning leftover, and it adopts dipping by lye wet blue waste material 36-48 hour, and swelling wet blue waste material is processed to 20-30 minute with ultrasonic equipment; Then, wet blue waste material is slowly passed through to high-voltage water jet device; Then dry, finally by further strike and the shredding of crossing carding machine, make thoroughly to produce and separate between collagenous fibres, obtain collagenous fibres.
Prior art is mainly that the mode of the processing that combines by physics, chemistry or physics and chemistry makes collagenous fibres loose in leather, is aided with subsequent treatment and makes it separate and obtain. adopt after chemical treatment the mode in conjunction with physical treatment again, as pickling swelling, alkalescence swollen, enzyme processing etc. easily makes collagenous fibres under chemical environment, occur to soften or overgenerous chemical environment makes tropocollagen molecule destructurized, expose combinative end group or be broken into little molecular radical, produce fibre debris, the active force producing through follow-up physical treatment is again larger, cause fibrillation impaired, having reduced can conjugated group, make in the time of the production of the preparation for yarn and fabric, easily produce adhesion deficiency, cause formed leather tension force inequality, easily scratch, the defects such as fracture, be not suitable for processing and the production of high-end real leather products, the fibre debris producing also runs off along with process, has caused the waste of resource, has improved the production cost of target product.
Summary of the invention
The object of this invention is to provide a kind of can direct spinning by the preparation method of collagenous fibres, the polar solvent that hydroxyl is rich in the method utilization is pretended use, in conjunction with the mode of ultrasonic processing, under condition as mild as a dove, realize dissociating of intermolecular high crystallization hydrogen bond, obtain loosely organized raw material, through rotary drum, processing eases back, liquid solution fibre, fiber is dried, again by the electric pulse processing in conjunction with suitable intensity under nitrogen protection condition of the collagenous fibres of the ultimate fibre state after drying, can increase fine fibre surface roughness, increase its binding ability in subsequent handling, fungistatic effect, preparation process cleanliness without any pollution, the collagenous fibres that make are without through graft modification or compoundly can directly adopt existing spinning technique to carry out spinning, the collagenous fibres that adopt the method to prepare carry out spinning, are woven into base cloth, the corium fabric leather that reprocessing forms has advantages of that tensile strength is high, wear-resisting, soft, moisture absorption, oil suction, easily dye, fire resistance is good, is particularly suitable for the production of high-end leather and fur products.
Another object of the present invention is to provide a kind of collagenous fibres that utilize above-mentioned preparation method to extract and obtain to prepare the method for corium fabric leather.
First object of the present invention is achieved through the following technical solutions: a kind of can direct spinning by the preparation method of collagenous fibres, be following steps:
(1) shear: taking wet blue leather as raw material, be cut into the size of production or equipment requirement with leather cutter;
(2) ultrasonic pretreatment: 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, regulating pH is 7 ~ 7.5, be warming up to 40 ~ 50 DEG C, the wet blue leather cutting is placed in one and is soaked 12 ~ 24 hours, then pretreatment fluid is warming up to 50 ~ 60 DEG C, regulating pH is 7.5 to 8, soak again 1 ~ 2 hour, under Current Temperatures, carrying out ultrasonic low frequency vibrates in short-term, the Ultrasonic Conditions adopting is: frequency 20 ~ 50kHz, power 200 ~ 600W, ultrasonic time 10 ~ 20 minutes; Wherein, the pretreatment fluid that is rich in the polar solvent of hydroxyl described in is according to volume ratio 1:(1 ~ 5 by the alkaline solution of mass concentration 2 ~ 10% and the alcoholic solution of mass concentration 45 ~ 75%) mix and make;
(3) rotary drum processing: ultrasonic pretreatment finishes, elimination pretreatment fluid, pretreated wet blue leather is adopted to rotary drum treatment process, first in aqueous environment, rotate rotary drum, 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 gradually softening agent amino silicon oil emulsion or ternary polymerization silicone oil emulsion, slowly rotate after rotary drum mixing fully, then rotate again the rotary drum processing 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 easing back through rotary drum processing, preliminary shredding is proceeded to liquid fiber uncoiling machine, and the centrifugal force producing by hydraulic mixing, separates collagenous fibres with textile fabric form; Then by dryer, the collagenous fibres of separating from liquid fiber uncoiling machine are being dried to indoor oven dry, the mode that furnace drying method adopts exhausting and air intake to combine, adopt exhausting as indoor in baking by being carried by air intake mode again after dry humid air extraction indoor baking, so loop oven dry, until the moisture 25 ~ 35% of fiber, the bake out temperature that adopts is 70 ~ 80 DEG C;
(5) shredding removal of impurities, combing: adopt opening to carry out shredding the fiber after drying, shredding method is, be to carry out shredding processing under Φ 380mm, the rotating speed parameter that is 600rpm at plucker roller diameter, and removed the impurity beyond fiber, obtain bunchy collagenous fibres; By carding machine, the collagenous fibres of bunchy are carded to the collagenous fibres of ultimate fibre state again, the design parameter on carding machine is, temperature is that 27 DEG C, humidity are 70%-75%, to go out net spee be 3.5m/min;
(6) fiber surface processing: the collagenous fibres that step (5) is 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 one or more the combination in ethanolic solution, isopropyl alcohol, n-butanol, propane diols, polyglycol solution.
The consumption of pretreatment fluid is as the criterion with the pending wet blue leather raw material of submergence completely. 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 part moisture, need to reuptake moisture, therefore, carrying out before ultrasonic pretreatment, also can be first wet blue leather raw material be immersed in pond 2 ~ 5 minutes, dry to moisture content 60 ~ 80% and carry out again ultrasonic pretreatment, the method both can wash away impurity, can also adjust the moisture of raw material, be conducive to after fiber water suction, while being conducive to follow-up ultrasonic processing, pretreatment fluid produces good osmosis by concentration difference, enters into the intermolecular dissociation to intermolecular crystal type hydrogen bond better.
Taking the operating environment of rotary drum as water, be convenient to add softening agent, make wet blue leather accelerate to ease back, by the mechanism of rotary drum, wet blue leather obtains preliminary shredding; Can also pretreatment fluid residual fibrous inside be cemented out by modes of action such as cleaning, difference in height, concentration differences in rotary drum processing procedure, avoid residual pretreatment fluid to impact fibre structure, thereby affect subsequent handling and product quality simultaneously; Described softening agent can adopt as softening agents such as amino silicon oil emulsion, ternary polymerization silicone oil emulsions, be combined with leather fiber by the amino in softening agent, hydroxyl, polyether group, can form the molecular layer that Si-O-Si finishes at fiber surface, produce soft, smooth feel, and ability selects the softening agent of different activities group to process as required, obtains the leather fiber of hydrophilic or hydrophobic effect.
Step (4) is described when fiber is dried, dryer can adopt Steam Heating, and compressor flow can adopt 15000 ~ 20000m3/h, and the collagenous fibres that collecting is bled takes away are to be back to production, particulate collagenous fibres dust enters dust collecting system, takes out in paper mill.
For ease of combing, fiber requires to have certain degree of opening, fiber after oven dry normally presents is entangled with into large bulk, can become fritter and then become fiber bundle-like by shredding program, then pass through carding machine, the collagenous fibres of bunchy are carded to ultimate fibre state, form the fleece of certain width, certain mass area ratio. When described removal of impurities, adopt dust collecting system to collect fiber grain, take out in paper mill, the collagenous fibres that obtain after removal of impurities can mix in proportion and make it homogenising according to need of production classification or by the collagenous fibres that length, fineness etc. there are differences large percentage.
The collagenous fibres length 5 ~ 50mm that adopts technique scheme to obtain, 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 that adopts the be directly used in spinning of first technical scheme acquisition of the present invention, when preparation, the collagenous fibres preparation that first can be directly used in spinning adopts spinning process spun yarn, weaves base cloth, then by soft through dyeing, be dried, drawing base cloth, flour milling, after arrange and make; Staining procedure is in conjunction with ultrasonic wave processing in the time carrying out for described dyeing process, and the ultrasonic wave treatment conditions that adopt are as follows: frequency 20 ~ 50kHz, power 200 ~ 600W, ultrasonic time 10 ~ 20 minutes; Described being dried is at 30 ~ 60 DEG C, to carry out micro-wave vacuum.
In above-mentioned technical scheme, described spinning process can be according to the different size of obtained collagenous fibres and produce the different requirements to yarn, select to adopt applicable spinning process, as traditional handicrafts such as ring spinning, air-jet spinning, friction spun yarns, or new spinning process, as new technologies such as air stream spinning, dry method spinning. Described afterfinish method also can adopt synthetic leather rear section method for sorting to carry out.
Adopt technique scheme, in the time of dyeing, collagenous fibres base cloth through dyestuff in the absorption on base cloth surface, to the three phases of base cloth internal layer diffusion, set on base cloth, by adopting ultrasonic wave can make collagenous fibres that the absorption of non-location occurs, increase dyeing affinity, increase colorant dissolubility, make fiber surface that similar etching effect occur; The dye granule of the phenomenons such as ultrasonic wave processing can also make easily to assemble, sedimentation resolves into uniform dispersion, improves diffusion, the seepage velocity of dyestuff; Ultrasonic wave is also processed and can the gas molecule that dissolve or be trapped in basic intertwined point, fiber capillary and gap location be expelled to solution by degasification, and get rid of thereupon, can make the attenuation of stickiness block layer by diffusion, be conducive to accelerate dye solution and be diffused into fibrous inside.
The dry run of technique scheme can be passed through the vacuum radiation heat effect of microwave, reaches painting cloth solid form, the object of fixing base cloth internalization work material. Painting cloth after microwave drying easily produces the phenomenons such as plate is hard, warpage, by drawing soft stretching, extension, makes fiber loose soft, high resilience, and the smooth softness of painting cloth of acquisition, without curling, area slightly increases.
Draw after the painting cloth stretching, extension of soft rear acquisition, can expose surperficial nibs, can eliminate such flaw by flour milling, assist uniform thickness, improve the physical property of painting cloth, prepare for covering with paint, lacquer, colour wash, etc.
By adopting and add auxiliary agent 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, for example increase its health care, as comprise 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, the dress of inflammable and explosive place.
The preparation method of collagenous fibres of the present invention passes through to adopt the cooperation processing of the key technology techniques such as the electric pulse processing of the suitable intensity of combination under polar solvent, ultrasonic pretreatment, nitrogen protection condition, as follows with respect to the beneficial effect of prior art:
(1) by adopting the macromolecular intermolecular hydrogen bonding of polar solvent resolution, embed little molecule polyphenol, be compounded to form new molecular association body by hydrogen bond again, this mode can make full use of be rich in hydroxyl polar solvent pretend use, under condition as mild as a dove, realizing the dissociating of high crystallization hydrogen bond, is a kind of green chemistry process route; Simultaneously by the variation of two stage different pH value, can more effective performance be rich in hydroxyl polar solvent pretend use;
(2) by rotary drum softening process step by step, can make the effect of supple-settlement significantly improve;
(3) ultrasonic processing pretreatment produces cavitation, makes molecular structure loose, and the fracture and the little molecule polyphenol that are conducive to later stage intermolecular hydrogen bonding enter in the middle of molecular structure, form stable molecular association body; The fractionation of polar solvent to macromolecular intermolecular hydrogen bonding also accelerated in ultrasonic pretreatment, and Reaction time shorten, enhances productivity;
(4) the suitably electric pulse processing of intensity of combination under nitrogen protection condition, can increase fine fibre surface roughness, increase its interfibrous adhesion in follow-up spinning process, formation has the base cloth of sufficient intensity, to improve mar proof, scratch resistance and the binding strength of corium fabric leather finished product; Electric field pulse is processed and can also after fibrocyte perforate membrane, the moisture that is trapped in fibrocyte inside be discharged, and also has the effect of sterilization simultaneously, and the collagenous fibres of preparation are played a protective role, and reduces the antibacterial cost of real leather products.
Wet blue leather of the present invention refer to animal hides leather through deoiling, degrease, depilation, chrome tanning contain certain moisture after processing, 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 as the animal of 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 be different from main employing needle point method as reinforcing means, account for 40～60% mixed fibre and make the method for non-weaving cloth fibrillation making synthetic leather base with extraction fiber, also be different from and will after leftover bits and pieces dissolving, carry out spinning, and then carry out the method for rear road processing. Corium fabric leather of the present invention is from wet blue leather, to extract the collagenous fibres that can be directly used in spinning to be prepared, the extraction process feature of environmental protection of its collagenous fibres is strong, the collagenous fibres that obtain have very strong adhesion and good physical characteristic, prepared corium fabric leather can be realized industrialized standard by the standard area of every leather 1.5m × 1.5m and produce, the various defects such as animal's leather tension force is irregular, easy scratch are well overcome, the preparation of very suitable high-end real leather products.
Brief description of the drawings
After Fig. 1 is collagenous fibres Direct Spinning resultant yarn of the present invention, then the configuration of surface (atomic force microscope images) of the fabric becoming with the weaving yarns being spun into, wherein Fig. 1 a is graphics, Fig. 1 b is phase diagram.
Detailed description of the invention
Below by embodiment, the present invention is described in further details, these embodiment are only used for illustrating the present invention, do not limit the scope of the invention.
Embodiment 1 adopts following steps to prepare a kind of collagenous fibres that are directly used in spinning:
(1) shear: taking wet blue leather as raw material, be cut into the size of production or equipment requirement with leather cutter;
(2) ultrasonic pretreatment: prepare pretreatment fluid, regulating pH is 7 ~ 7.5, heat up 40 ~ 50 DEG C, the wet blue leather cutting is immersed in to pretreatment fluid completely and soaks 12-24 hour, then pretreatment fluid is warming up to 50-60 DEG C, regulating pH is 7.5 to 8, soak 1-2 hour again, carry out ultrasonic low frequency and vibrate in short-term under Current Temperatures, the Ultrasonic Conditions adopting 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 and make;
(3) rotary drum processing: ultrasonic pretreatment finishes, elimination pretreatment fluid, pretreated wet blue leather is adopted to rotary drum treatment process, first in aqueous environment, rotate rotary drum, 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 gradually softening agent ternary polymerization silicone oil emulsion, slowly rotate after rotary drum mixes fully, more then rotate the rotary drum processing that eases back, 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 easing back through rotary drum processing, preliminary shredding is proceeded to liquid fiber uncoiling machine, and the centrifugal force producing by hydraulic mixing, separates collagenous fibres with textile fabric form; Then by dryer, the collagenous fibres of separating from liquid fiber uncoiling machine are being dried to indoor oven dry, the mode that furnace drying method adopts exhausting and air intake to combine, adopt exhausting as indoor in baking by being carried by air intake mode again after dry humid air extraction indoor baking, so loop oven dry, until the moisture 25 ~ 35% of fiber, the bake out temperature that adopts is 70 ~ 80 DEG C;
(5) shredding removal of impurities, combing: adopt opening to carry out shredding the fiber after drying, shredding method is, be to carry out shredding processing under Φ 380mm, the rotating speed parameter that is 600rpm at plucker roller diameter, and removed the impurity beyond fiber, obtain bunchy collagenous fibres; By carding machine, the collagenous fibres of bunchy are carded to the collagenous fibres of ultimate fibre state again, the design parameter on carding machine is, temperature is that 27 DEG C, humidity are 70%-75%, to go out net spee be 3.5m/min;
(6) fiber surface processing: the collagenous fibres that step (5) is 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 that are directly used in spinning:
(1) shear: taking wet blue leather as raw material, be cut into the size of production or equipment requirement with leather cutter;
(2) ultrasonic pretreatment: the polar solvent pretreatment fluid of hydroxyl is rich in preparation, regulating pH is 7, be warming up to 45 DEG C, the wet blue leather cutting be immersed in to pretreatment fluid completely and soak 24 hours, then pretreatment fluid is warming up to 50 DEG C, regulating pH is 7.5 to 8, soak 2 hours again, carry out ultrasonic low frequency and vibrate in short-term under Current Temperatures, the Ultrasonic Conditions adopting is: frequency 20kHz, power 200W, ultrasonic time 20 minutes; Pretreatment fluid is to be mixed and make according to volume ratio 1:1 by the sodium hydroxide solution of mass concentration 2% and the polyglycol solution of mass concentration 75%;
(3) rotary drum processing: ultrasonic pretreatment finishes, elimination pretreatment fluid, pretreated wet blue leather is adopted to rotary drum treatment process, first in aqueous environment, rotate rotary drum, 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 gradually softening agent amino silicon oil emulsion, slowly rotate after rotary drum mixes fully, more then rotate the rotary drum processing that eases back, 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 fibre, fiber are dried: the wet blue leather easing back through rotary drum processing, preliminary shredding is proceeded to liquid fiber uncoiling machine, and the centrifugal force producing by hydraulic mixing, separates collagenous fibres with textile fabric form; Then by dryer, the collagenous fibres of separating from liquid fiber uncoiling machine are being dried to indoor oven dry, the mode that furnace drying method adopts exhausting and air intake to combine, adopt exhausting as indoor in baking by being carried by air intake mode again after dry humid air extraction indoor baking, so loop oven dry, until the moisture 30% of fiber, the bake out temperature that adopts is 75 DEG C;
(5) adopt opening to carry out shredding the fiber after drying, shredding method is, is to carry out shredding processing under Φ 380mm, the rotating speed parameter that is 600rpm, and removed the impurity beyond fiber at plucker roller diameter, obtains bunchy collagenous fibres; By carding machine, the collagenous fibres of bunchy are carded to the collagenous fibres of ultimate fibre state again, the design parameter on carding machine is, temperature is that 27 DEG C, humidity are 75%, to go out net spee be 3.5m/min;
(6) fiber surface processing: the collagenous fibres that step (5) is 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 that are directly used in spinning:
(1) shear: taking wet blue leather as raw material, be cut into and produce or the size of equipment requirement with leather cutter, wet blue leather raw material is immersed in pond 2 ~ 5 minutes, dry to moisture content 60 ~ 80%;
(2) ultrasonic pretreatment: prepare pretreatment fluid, regulating pH is 7, be warming up to 50 DEG C, wet blue leather be immersed in to pretreatment fluid completely and soak 12 hours, then pretreatment fluid is warming up to 55 DEG C, regulating pH is 7.5, soak 1.5 hours again, carry out ultrasonic low frequency and vibrate in short-term under Current Temperatures, the Ultrasonic Conditions adopting is: frequency 40kHz, power 600W, ultrasonic time 10 minutes; Pretreatment fluid is to be mixed and make according to volume ratio 1:5 with mixed with propylene glycol solution (isopropyl alcohol is 2:3 with propane diols volume ratio) by the sodium hydroxide solution of mass concentration 10% and the isopropyl alcohol of mass concentration 45%;
(3) rotary drum processing: ultrasonic pretreatment finishes, elimination pretreatment fluid, pretreated wet blue leather is adopted to rotary drum treatment process, first in aqueous environment, rotate rotary drum, 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 gradually softening agent amino silicon oil emulsion, slowly rotate after rotary drum mixes fully, more then rotate the rotary drum processing that eases back, 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 fibre, fiber are dried: the wet blue leather easing back through rotary drum processing, preliminary shredding is proceeded to liquid fiber uncoiling machine, and the centrifugal force producing by hydraulic mixing, separates collagenous fibres with textile fabric form; Then by dryer, the collagenous fibres of separating from liquid fiber uncoiling machine are being dried to indoor oven dry, the mode that furnace drying method adopts exhausting and air intake to combine, adopt exhausting as indoor in baking by being carried by air intake mode again after dry humid air extraction indoor baking, so loop oven dry, until the moisture 35% of fiber, the bake out temperature that adopts is 70 DEG C;
(5) adopt opening to carry out shredding the fiber after drying, shredding method is, is to carry out shredding processing under Φ 380mm, the rotating speed parameter that is 600rpm, and removed the impurity beyond fiber at plucker roller diameter, obtains bunchy collagenous fibres; By carding machine, the collagenous fibres of bunchy are carded to the collagenous fibres of ultimate fibre state again, the design parameter on carding machine is, temperature is that 27 DEG C, humidity are 70%, to go out net spee be 3.5m/min;
(6) fiber surface processing: the collagenous fibres that step (5) is 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 that are directly used in spinning:
(1) shear: taking wet blue leather as raw material, be cut into the size of production or equipment requirement with leather cutter;
(2) ultrasonic pretreatment: prepare pretreatment fluid, regulating pH is 7.5, heat up 40 DEG C, the wet blue leather cutting is immersed in to pretreatment fluid completely and soaks 20 hours, then pretreatment fluid is warming up to 60 DEG C, regulating pH is 7.5, soak 1 hour again, carry out ultrasonic low frequency and vibrate in short-term under Current Temperatures, the Ultrasonic Conditions adopting is: frequency 50kHz, power 400W, ultrasonic time 15 minutes; Pretreatment fluid is to be mixed and make according to volume ratio 1:3 by the sodium hydroxide solution of mass concentration 5% and the polyglycol solution of mass concentration 50%;
(3) rotary drum processing: ultrasonic pretreatment finishes, elimination pretreatment fluid, pretreated wet blue leather is adopted to rotary drum treatment process, first in aqueous environment, rotate rotary drum, 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 gradually softening agent ternary polymerization silicone oil emulsion, slowly rotate after rotary drum mixes fully, more then rotate the rotary drum processing that eases back, 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 easing back through rotary drum processing, preliminary shredding is proceeded to liquid fiber uncoiling machine, and the centrifugal force producing by hydraulic mixing, separates collagenous fibres with textile fabric form; Then by dryer, the collagenous fibres of separating from liquid fiber uncoiling machine are being dried to indoor oven dry, the mode that furnace drying method adopts exhausting and air intake to combine, adopt exhausting as indoor in baking by being carried by air intake mode again after dry humid air extraction indoor baking, so loop oven dry, until the moisture 25% of fiber, the bake out temperature that adopts is 80 DEG C;
(5) shredding removal of impurities, combing: adopt opening to carry out shredding the fiber after drying, shredding method is, be to carry out shredding processing under Φ 380mm, the rotating speed parameter that is 600rpm at plucker roller diameter, and removed the impurity beyond fiber, obtain bunchy collagenous fibres; By carding machine, the collagenous fibres of bunchy are carded to the collagenous fibres of ultimate fibre state again, the design parameter on carding machine is, temperature is that 27 DEG C, humidity are 75%, to go out net spee be 3.5m/min;
(6) fiber surface processing: the collagenous fibres that step (5) is 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 5 gets the collagenous fibres preparation of the be directly used in spinning that embodiment 1 prepares and prepares as follows corium fabric leather: the collagenous fibres preparation of getting the be directly used in spinning that embodiment 1 prepares adopts RING SPINNING spinning process spun yarn, weave base cloth, again by the dyeing of base cloth process, at 50 DEG C, carry out micro-wave vacuum dry, staking machine draws soft, flour milling, add finishing agent, mould inhibitor, fire retardant carries out rear arrangement and makes, dyeing process in the time carrying out staining procedure in conjunction with ultrasonic wave processing, the ultrasonic wave treatment conditions that adopt are as follows: frequency 30kHz, power 500W, ultrasonic time 15 minutes.
Claims (7)
1. can direct spinning by the preparation methods of collagenous fibres, it is characterized in that: adopt following steps:
(1) shear: taking wet blue leather as raw material, be cut into the size of production or equipment requirement with leather cutter;
(2) ultrasonic pretreatment: 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, regulating pH is 7 ~ 7.5, be warming up to 40 ~ 50 DEG C, the wet blue leather cutting is placed in one and is soaked 12 ~ 24 hours, then pretreatment fluid is warming up to 50 ~ 60 DEG C, regulating pH is 7.5 to 8, soak again 1 ~ 2 hour, under Current Temperatures, carrying out ultrasonic low frequency vibrates in short-term, the Ultrasonic Conditions adopting is: frequency 20 ~ 50kHz, power 200 ~ 600W, ultrasonic time 10 ~ 20 minutes; Wherein, the pretreatment fluid of the described polar solvent that is rich in hydroxyl is according to volume ratio 1:(1 ~ 5 by the alkaline solution of mass concentration 2 ~ 10% and the alcoholic solution of mass concentration 45 ~ 75%) mix and make, described aqueous slkali is one or both the combination in sodium hydroxide solution, sodium bicarbonate solution, and described alcoholic solution is one or more the combination in ethanolic solution, isopropyl alcohol, n-butanol, propane diols, polyglycol solution;
(3) rotary drum processing: ultrasonic pretreatment finishes, elimination pretreatment fluid, pretreated wet blue leather is adopted to rotary drum treatment process, first in aqueous environment, rotate rotary drum, 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 gradually softening agent amino silicon oil emulsion or ternary polymerization silicone oil emulsion, slowly rotate after rotary drum mixing fully, then rotate again the rotary drum processing 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 easing back through rotary drum processing, preliminary shredding is proceeded to liquid fiber uncoiling machine, and the centrifugal force producing by hydraulic mixing, separates collagenous fibres with textile fabric form; Then by dryer, the collagenous fibres of separating from liquid fiber uncoiling machine are being dried to indoor oven dry, the mode that furnace drying method adopts exhausting and air intake to combine, adopt exhausting as indoor in baking by being carried by air intake mode again after dry humid air extraction indoor baking, so loop oven dry, until the moisture 25 ~ 35% of fiber, the bake out temperature that adopts is 70 ~ 80 DEG C;
(5) shredding removal of impurities, combing: adopt opening to carry out shredding the fiber after drying, shredding method is, be to carry out shredding processing under Φ 380mm, the rotating speed parameter that is 600rpm at plucker roller diameter, and removed the impurity beyond fiber, obtain bunchy collagenous fibres; By carding machine, the collagenous fibres of bunchy are carded to the collagenous fibres of ultimate fibre state again, the design parameter on carding machine is, temperature is that 27 DEG C, humidity are 70%-75%, to go out net spee be 3.5m/min;
(6) fiber surface processing: the collagenous fibres that step (5) is obtained are placed in impulse electric field and carry out surface treatment under nitrogen protection condition; making 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: carrying out before ultrasonic pretreatment, first wet blue leather raw material is immersed in pond 2 ~ 5 minutes, dry to moisture content 60 ~ 80% and carry out ultrasonic pretreatment again.
3. preparation method according to claim 1, is characterized in that: the consumption of described pretreatment fluid is soaking completely
Do not have pending wet blue leather raw material to be as the criterion.
4. preparation method according to claim 1, is characterized in that: step (4) is described when fiber is dried, and dryer adopts Steam Heating, compressor flow 15000 ~ 20000m3/h.
5. preparation method according to claim 1, is characterized in that: what adopt that this preparation method obtains 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: adopt the collagenous fibres preparation of the be directly used in spinning of preparation method's acquisition of claim 1, when preparation, the collagenous fibres preparation that first can be directly used in spinning adopts spinning process spun yarn, weaves base cloth, then by soft through dyeing, be dried, drawing base cloth, flour milling, after arrange and make; Staining procedure is in conjunction with ultrasonic wave processing in the time carrying out for described dyeing process, and the ultrasonic wave treatment conditions that adopt are as follows: frequency 20 ~ 50kHz, power 200 ~ 600W, ultrasonic time 10 ~ 20 minutes; Described being dried is at 30 ~ 60 DEG C, to carry out micro-wave vacuum.
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| 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 |
| 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 |
| CN107227628A (en) * | 2017-07-03 | 2017-10-03 | 徐琦 | The method for going back raw hide is prepared based on collagen fabric fabric combination flocking technique |
| 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 |
| CN107237177A (en) * | 2017-07-03 | 2017-10-10 | 徐琦 | Multifunctional fabric prepared based on collagen fabric fabric and preparation method thereof |
| CN107385948B (en) * | 2017-07-03 | 2018-09-28 | 徐琦 | The method for going back raw hide is prepared based on collagen fabric fabric combination water jet process |
| CN108251905B (en) * | 2018-01-19 | 2019-05-28 | 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 |
| CN113106594B (en) | 2019-05-27 | 2022-03-25 | 广东五源新材料科技集团有限公司 | Product with nano-grade branch animal leather fiber bundle |
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| CN102286790B (en) * | 2011-06-02 | 2012-12-26 | 沈中全 | Preparation method of leather flocking short fiber |
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