CN101512051A - Process for producing nanofibers - Google Patents
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- CN101512051A CN101512051A CNA2007800321528A CN200780032152A CN101512051A CN 101512051 A CN101512051 A CN 101512051A CN A2007800321528 A CNA2007800321528 A CN A2007800321528A CN 200780032152 A CN200780032152 A CN 200780032152A CN 101512051 A CN101512051 A CN 101512051A
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Abstract
A process for making nanofibers includes preparing a fluid suspension of fibers, shear refining the fibers to create fibrillated fibers, and subsequently closed channel refining or homogenizing the fibrillated fibers to detach nanofibers from the fibrillated fibers. The shear refining of the fibers in the fluid suspension generates fiber cores having attached nanofibers. The closed channel refining or homogenizing of the fibrillated fibers is initially at a first shear rate and, subsequently, at a second, higher shear rate, to detach nanofibers from fiber cores and to create additional nanofibers from the fiber cores. The fiber suspension may flow continuously from the shear refining to the closed channel refining or homogenizing, and include controlling the rate of flow of the fiber suspension from the shear refining to the closed channel refining or homogenizing.
Description
Technical field
The present invention relates to the manufacture method of fiber, relate in particular to the manufacture method of nano-scale fiber.
Background technology
At United States Patent(USP) Nos. 2,810, the manufacture process of known fibrillating fibre in 646,4,495,030,4,565,727,4,904,343,4,929,502 and 5,180,630.The method that is used for making this fibrillating fibre has comprised that utilization is at the papermaking machine of industry and the agitator of industry.In various application, need under low-cost situation, efficiently produce the fiber of nano-scale in batches, but the method and apparatus of prior art can not be realized such purpose effectively.
Summary of the invention
Therefore, consider prior art problems and defective, the object of the present invention is to provide a kind of manufacturing nano-scale fiber and fibriilar improvement processing method and system.Another object of the present invention is to provide a kind of method and system of making the nano-scale fiber, and this nano-scale fiber has reduced the fibre core that is blended in wherein in a large number.
Another purpose of the present invention just has bigger uniformity and flowability providing a kind of manufacturing to have to improve the method and system of the nano-scale fiber of characteristic.
One object of the present invention is to provide a kind of method and system of making the nano-scale fiber, and they utilize energy and have more production capacity than prior art is more effective, and produce volume and the output that improves.
Other purposes of the present invention and advantage will become from specification, and part is known and part is obvious.
Obvious for those skilled in the art above-mentioned and other purposes will realize in the present invention, the invention provides a kind of method of making nanofiber, it comprises the suspension of preparing fiber, shear this fiber of refining to produce fibrillating fibre, and close stream refining or homogenising fibrillating fibre subsequently, from fibrillating fibre, to separate nanofiber.The shearing refining process of fiber produces and to have the fibre core of attached nanofibers in suspension, and closes the stream refining or the homogenising process is separated nanofiber from fibre core.This fibrous suspension will flow to from the shearing refining process continuously and close stream refining or homogenising process, and comprise that control is from shearing refining process to the flow rate of closing fibrous suspension stream refining or the homogenising process.
This process also further comprises from remaining formation isolates the nanofiber that this has separated the fibriilar or core fibre in large quantities.This closes the stream refining or the homogenising process will continue, additionally to produce nanofiber from the residual fiber core.
Close in the stream refining process in employing, carry out with first shear rate at first, and implement to separate nanofiber in the leaf fibre core with the second higher shear rate subsequently, and from this fibre core, produce other nanofiber from fibrillating fibre.It can be to shear, crushing, pat and the cutting fibrillating fibre that fibrillating fibre this closes the stream refining.
This process also comprises removing to be sheared refining, is closing the heat that produces in the fibrous suspension during stream refining or the homogenising process.In yet another aspect, the invention provides a kind of method of making nanofiber, it comprises that preparation comprises the suspension of the fibrillating fibre of fibre core, wherein this fibre core has the nanofiber that adheres to, under first shear rate, close stream refining or homogenising fibrillating fibre at first, from fibre core, separate nanofiber with the second higher shear rate subsequently, and from this fibre core, produce other nanofiber.This fibrous suspension flow to second rotor that second shear rate is moved from the first rotor of first shear rate operation, and preferred flow is continuously and connects.This process also comprises the flow rate of controlling fiber suspension.Implement to close the stream refining process by the fibrous suspension between the tooth that moves each other, the tooth that separates is implemented in the fiber of sufficient shearing force in fibrous suspension, to separate nanofiber and optionally produce other nanofiber from fibrillating fibre from fibre core.The homogenising process can be implemented by following process, pass through the hole of a size by the fibrous suspension that fibrous suspension is pressurizeed and will pressurize, and under a pressure, implement in the enough fiber of shearing force in fibrous suspension, from fibrillating fibre, to separate nanofiber and from fibre core, optionally to produce other nanofiber.In yet another aspect, the present invention relates to a kind of fibre composition, it comprises the mixture of fibre core and the nanofiber that separates from fibre core, this fibre core has the length of diameter and the about 0.1-6mm of about 500-5000nm, and nanofiber has the length of diameter and the about 0.1-6mm of about 50-500nm.The invention still further relates to a kind of fibre composition, it comprises the nanofiber that breaks away from substantially from fiber, and this nanofiber has the length of diameter and the about 0.1-6mm of about 50-500nm.
The accompanying drawing summary
Feature of the present invention is thought novel and component feature of the present invention will elaborate from additional claim.These accompanying drawings only are purposes of illustration, rather than describe in proportion.Yet in detailed description with the accompanying drawing, the present invention self comprises the understanding that structure and operation method will be better.
Fig. 1 is the side view in cross section of optimum decision system that is used to produce the keying stream refiner of nanofiber according to the present invention.
Fig. 2 is the top plan view of partial cross section of refining agent rotor of the open circuit of Fig. 1.
Fig. 3 is the top plan view that first of Fig. 1 closes the refining agent of stream, and it produces low-level relatively shearing refining process.
Fig. 4 is the rotor portion of the refiner that closes stream of Fig. 3, the side view of part cross section.
Fig. 5 is the side view that second of Fig. 1 closes the refining agent of stream, and it produces high-caliber relatively shearing refining process.
Fig. 6 is the rotor of the refiner that closes stream of Fig. 5 and the top plan view of stationary part.
Fig. 7 is the cutaway view of homogenising unit, and it can use or replace it with the stream refiner that closes of Fig. 3 in the system of Fig. 1-6.
Fig. 8 is the microphoto with fibriilar fiber of nano-scale.
Fig. 9 shows the microphoto of the nanofiber that separates according to the present invention from fibre core.
The microphoto that has gone out the nanofiber that separates from fibre core according to the present invention and from fibre core, rupture that Figure 10 is.
Specific implementation method
In describing the process of the preferred embodiments of the present invention, at this referring to accompanying drawing 1-10, wherein identical numeral feature of the present invention.The invention provides a kind of machining, be used for multiple use, produce the fibriilar effective ways of nano-scale fiber by batch by fiber.This term ＂ ＂ fiber ＂ means that the high aspect ratio with the length diameter group is the entity of feature.For example, in nanofiber production process according to the present invention, can utilize from greater than about 2 to the aspect ratio of about length more than 1000 than average diameter.This term ＂ fibrillating fibre ＂ is meant to have the splintery fibrillation that distributes along fibre length, and has about 2 to about 100 length-width ratio and less than the fiber of about 1000 nanometer diameters.The fibrillating fibre that extends from fiber is commonly referred to ＂ core fibre ＂, has remarkable diameter less than the core fibre that extends from fibrillation.The fibrillation that extends from core fibre preferably has the diameter less than the nanofiber range of about 1000 nanometers.As used herein, the term nanofiber means a kind of fiber, no matter extends or separates from core fibre from core fibre, has the diameter less than about 1000 nanometers.The mixture of nanofibers that produces from the present invention has about 50 nanometers usually to the diameter less than about 1000 nanometers, and the length of 0.1-6mm.Nanofiber has the diameter of about 50-500 nanometer, and the length of 0.1-6mm.
The initial step of producing nanofiber is to produce to have fibre core and the fibriilar fibrillating fibre of additional nanometer.Produce this fibrillating fibre by shearing fibre in the described method in the prior art, this shear history can comprise that refining, crushing, beating, cutting, mechanical agitation and high shear mix process.Selectable, by identical inventor, the U.S. Patent application no.[atty.docket no.KXIN 100007000 that in same date, applies for], title is the process ＂ that ＂ produces fibrillating fibre, in the method for middle description, passes through shear history, there is not substantial crushing, pat and cutting, produce this fibrillating fibre, this application is carried out combination as a reference at this.This process is preferably included under first shear rate first open circuit refining fiber producing fibrillating fibre, and subsequently, open circuit refining fiber under second shear rate higher than first shear rate is to increase the original fiber degree of this fiber.The result of prior art or replaceable process is that fiber is broken down into fibre core and additional fibrillation, and need not cut this fibre core.As used herein, the refining of term open circuit is meant the physical process of fiber, and is main by shearing, and do not have substantial crushing, pats and cutting, and it causes the fibrillation process of the fiber limited reduction or meticulous manufacturing of fibre length.The substantial crushing of fiber, beating and working angles are not desirable in the manufacturing of filter element, for example, because this effect can cause the quick decomposition of fiber, and have many meticulous, in the production of low quality fibrillation of short fiber and pressing fiber, when being incorporated into paper filter, this fiber can provide the efficient filtration structure.The open circuit refining process also is called shear history, normally utilizes one or more that widen spacing or flat blade or plates, aqueous fibre suspension is handled implemented.The effect of single translational surface fully away from other surfaces, mainly applies on the fiber of shearing force in independent shearing field.Shear rate is different to the maximum shear value at the excircle place of blade or plate with near the low numerical value pivot or the rotating shaft, realizes that wherein maximal phase is to tip (circumferential) velocity (speed).Yet this shear force is low-down, when comparing with the shearing force that common surperficial method of refining produces, in the method, two approximating surfaces cause shearing fibre energetically, as at agitator, in cylindrical and quick runner refiner and the two disk refiners.The latter's example adopts a rotor, and it has the rotor of a row or multi-row tooth that rotates at a high speed in stator interior or relative stator.
Opposite, the term closed channel refining is meant the physical process of fiber, it causes the minimizing of fibrillation and the fiber size and the length of fiber by the combination of shearing, crushing, beating and cutting, and compares the meticulousr fiber of generation with the open circuit refining.Usually by in the beater of industry or taper shape or flat plate refiner, aqueous fibre suspension being used for implementing to close the stream refining process, in the latter, utilize the flat blade or the plate of the tight spacing that rotates together each other.This process is implemented under the situation below, and one of them blade or plate are static and another rotates, and perhaps two blades or plate are with different angular speed or different directions rotation.The action meeting of blade or plate surface both produces shearing force and other physical force on fiber, and each surface can be strengthened by another surperficial shearing force and cutting force that produces.As in the open circuit refining process, shear rate between relative rotating vane or plate, different with near the low numerical value pivot or rotating shaft to the maximum shear value at the excircle place of blade or plate, realize that at this excircle place maximal phase is to tip (circumferential) velocity (speed).
In a preferred embodiment of the invention, fibrillating fibre and nanofiber produce in the refiner of continuous stirring, adopt such as cellulose, polyolefin, polyester, nylon, the material manufacturing of aramid and liquid crystal polymer fibre, particularly polypropylene and polyethylene fiber.Usually, the fiber of Cai Yonging can be organic or inorganic material in the present invention, includes but not limited to condensate, engineering resin, pottery, cellulose, artificial silk, glass, metal, activated alumina, carbon or activated carbon, silica, zeolite or their combination.Can conceive the combination of organic and inorfil and/or fibrous crystal and within the scope of the invention, for example, glass, pottery or metal fibre and polymer fiber can use together.
The fibrillating fibre that the present invention produces and the quality of nanofiber adopt an important aspect, and Canadian standard freeness numbers is measured.Canadian Standard Freeness (CSF) means the numerical value of paper pulp freedom or rate of discharge, and its speed of being discharged by pulp suspension is measured.Those skilled in the art that the method is made the field for newspaper are known.Though the CSF value produces stronger susceptibility to fibre length generation susceptibility a little to fiber fibrillation and distribution of fiber diameters degree.Thereby, CSF, it is the measured value of the water easy degree of removing from paper pulp, is the proper method of monitoring fiber fibrillation and distribution of fiber diameters degree.If surface area is very big, this means many nanofibers and the fibriilar generation of nanometer on the surface of core fibre, then, few water will be discharged from paper pulp in measuring preset time, and when fiber more widely during fibrillation, the CSF value will become lower gradually.
After the manufacture process with fibre core and the fibriilar fibrillating fibre of additional nanometer, this fibrillating fibre is subjected to certain processing procedure then, to peel off from this core or other modes move this nanofiber.In the end in this stage, this can produce the mixing of nanofiber and bigger fibre core.Preferably, manufacturing of the present invention has the nanofiber of very small amount of this residual fiber core.This realizes by defibre core from nanofiber, for example, and by filtering or centrifuge, perhaps other sorting techniques.Selectable, also fibre core is further handled, preferably when still mixing with the nanofiber of originally peeling off, shear with the broken fiber core by closing stream, to produce other nanofiber, in this situation subsequently, the fibrillation of nanofiber is escaped further becoming meticulousr, because the still not enough cutting of the shearing force that applies and damage the little fibrillation that separates.Therefore, the present invention produces high-quality nanofiber, and can significantly not damage to become shorter whisker of low value or fines fibrillation.
Preferably, fibrillating fibre has 200 to 0, and perhaps 100 or lower CSF speed, and be subjected to two stage closed channel refining effects, from the pristine fibre core, to isolate nanofiber.The preferred phase I of closing the stream refining is low speed, high shear closed channel refining, and its back is high speed, high shear refining process.The fibrillating fibre of beginning is by weight the aqueous suspension of calculation in 0.1% to 25% concentration.In this phase I, nanofiber is peeled off from core fibre, and the further refining of core fibre.Then, the second level that preferably supplies under unusual high shear of this mixture of the nanofiber of separation and core fibre is closed in the stream refining process.Close stream between refining period in this second stage, the further refining of this fibre core to be producing more nanofiber, and can not influence the nanofiber that has separated in fact.Yet, consequent fibre blend turn back to the phase I close stream refining and/or second stage close the stream refining, and handle once more, be transformed into nanofiber, have the nanometer mud of the pristine fibre core that dwindles substantially with generation up to all fibres core basically.
The preferred continuous structure of open circuit and closed channel refiner is described in Fig. 1, and wherein refiner 70,90 and 100 in series illustrates.Refiner 70 is open channel refiner, and it has around a chuck of rotor 52, the housing 42 of water-cooled.Refiner 90 and 100 is closed channel refiner, and they have chuck respectively, the shell 63 of water-cooled and the rotor 62 and 72 of encapsulation.Other open channel refiner can in series be arranged on before the refiner 70.Each refiner has motor 46, and its axle 44 that is operably connected is equipped with blade, plate or rotor on this axle 44.This term rotor should alternately be used in blade or plate, unless otherwise mentioned.
Closed channel refiner 90 and 100 is being followed open channel refiner 70 in process order, the former preferred embodiment is shown in Fig. 3-6.Illustrate as more details in Fig. 3 and 4, low relatively shear closed channel refiner 90 is similar to the Valley beater, and the fibrous suspension 80 that reception is introduced is to the elliptical orbit 94 of shell 92 inside.Cylindrical rotor or beater 62 have the bar 64 of gear dentation beater, and it stretches out from circumference on the direction parallel with central shaft 44.Rotor 62 is gone up rotation in direction 97 (figure A), and forces pending fibrous suspension 81 between tooth or bar 64 and track, to realize closing stream, the desirable degree of high shear refining.The edge of the bar 64 by changing beater and the clearance distance x between the track, perhaps by being adjusted at the force value that is applied on the orbital direction on the rotor 62, the degree of shear that is applied to fiber in the suspension can be adjusted.Track 95 is bent upwards on the part of the circumference of rotor 62, and to increase the zone of using under the high shear forces power, after this, track 96 is crooked backward downwards, refluxes around direction 98 to allow fibrous suspension, to process once more by rotor 62.The part in the zone of the track 95 below rotor 62 can be by flexible, and rubber diaphragm is made.After processing reached required degree to fibrous suspension, its direction 82 from close stream refiner 90 withdrawed from.Usually at this moment, the fibrillation of original nanofiber separates from fibre core substantially, and fibre core self partly ftractures and is cut into the fiber of nano-scale.
Then, this fibrous suspension is also further handled closing in the stream refiner 100 of high shear, and more details are shown in Fig. 5 and 6.Refiner 100 can be similar to from NY, the Ross high-shear mixer that the Charles Ross and Son company of Hauppauge obtains, perhaps the Silverson blender that obtains from the Silverson Machines Co., Ltd of U.KChesham Bucks.Rotor 72 is driven to rotate in direction 79 (Fig. 6) with respect to static cylinder shape stator 76 by axle 44, and this stator 76 has a series of spaced apertures 78 around circumference, and the edge action of this stator is static tooth.The rotor 72 that illustrates has four arm or the teeth 73 that radially extend, and its end surface 74 and inner surface of stator are by a required gap y, and for example 0.050in (1.3mm) is spaced apart.Any combination of the number of rotor tooth and stator openings can be used to be implemented in the required high level of fiber shearing between rotor surface and the stator openings edge as required.Rotor and stator immerse a required period in the fibrous suspension of the housing that closes stream refiner 100 inside, with remaining fibre core cracking be cut into the fiber of nano-scale.The original nanofiber that produces in previous refining process is gone up substantially can not be subjected to the influence of high shear refiner 100 processing procedures subsequently.
In the rotation treatment facility, in the open circuit and closed channel refiner such as Fig. 1-6, by changing the structural design of rotor surface, the angular speed by increasing rotor or by increasing the diameter of rotor, the maximum shear stress at the excircle place of rotating vane or plate can obtain increasing.When the top speed of rotor increased, shear rate was increased to maximum from minimum.Optionally, by the suspension in the homogenising device being pressurizeed and forcing the suspension of pressurization to pass through less nozzle or hole, fibrous suspension is handled, further all substantially fibre cores are converted into nanofiber by cellular spliting.This homogenising effect makes fiber be subjected to high shear forces, and implements after one or two closes the said process that flows refiner, perhaps replaces such processing procedure.This homogenising device can use (for example, using in the back) with the stream refiner that closes of Fig. 3-6, and perhaps replaces them.As shown in Figure 7, homogenising device 110 (also being called the homogenising unit) is by preliminary treatment galvanic couple 112, and jet element 114 and absorptive unit are formed.This this fiber pulp 80 has CSF0 usually, under high pressure supplies in the upstream chamber of homogenising unit 116.This preliminary treatment galvanic couple is used for controlling fiber and enters cavitation before the nozzle.This fiber is dispersed in the pretreatment zone 112 preferably and nozzle 114 is passed through in effect.Can change with control viscosity this nozzle diameter, flow velocity, pressure and cavitation are so that produce optimum cellular spliting.Usually, nozzle diameter is 0.2mm.When fiber passed through nozzle, a very high shearing force was applied on the fiber.The Pressure control on the fiber pulp about 2000 and 45000psi (15 and 300Mpa) between.The slurry that comes out from nozzle enters the absorptive unit 116, illustrates to have the reactor 118 that each length is 2mm, and they are used for absorbing kinetic energy.After nozzle came out, cavitation can cause nanofiber to separate with core fibre in fiber pulp, and further core fibre was split into thinner fiber.In absorptive unit 116, kinetic energy is absorbed.The length of absorptive unit and diameter can change with control processing time and turbulent flow.The mud 84 that produces turns back to import, repeatedly to pass through the homogenising device.Also can be reverse inner flow direction of absorptive unit, producing more turbulent flow, this can make fiber separation in turn.
Turn back to Fig. 1, supply to open channel refiner 70, begin to make the process of fibrillating fibre by aqueous suspension with fiber.This original fiber has several microns diameter, and fibre length changes from 2-6mm.The concentration of fiber is calculated by weight to 1-6% in water.After open channel refiner 70, the feature of fibrillating fibre 80 adopts the Canadian Standard Freeness rate representation of fibre blend, and passes through measuring method.Usually, the fiber of beginning has about 750 to 700 CSF speed, and each stage along with refining drops to one about 400 to 0 preferred final CSF speed then.As shown in Figure 8, the fibrillating fibre product of the completion that obtains at the end of processing procedure has most nanofiber or still is attached to the fibrillation of core fibre.Supply with open channel refiner 70 fibers continuously, after required time of this open circuit refining, the suspension 80 preferred closed channel refiner 90 that flow to continuously subsequently of the fibrillating fibre that produces, wherein his closed circuit shearing under low relatively shear rate is to remove the nanofiber of attachment removal from fibre core.For example, at the spinner velocity of closed circuit refining place of phase I from 400-1800rev/min.Then, the fibrous suspension 82 of section processes closes stream refiner 100 from closing 90 inflows of stream refiner, and wherein in service at continuous mode, this fibrous suspension is further closed circuit refining under bigger shear rate.For example, at the spinner velocity of closed circuit refining place in the second level from about 400-3600rev/min.By the mixture that closes fibre core that flows the refining manufacturing and the nanofiber that separates with fibre core as shown in Figure 9.By increasing the speed of shearing, patting and cut, for example by increasing rotating speed or root diameter, perhaps time in refiner, closing the concise degree of stream obtains increasing,, and can the nanofiber that has separated not exerted an influence substantially producing more nanofiber with further refining fibre core.The nanofiber suspended matter 84 of this completion occurs from refiner 100.At the nanofiber in this stage, comprise the mixture of fibrillation that from fibre core, separates and the fiber that from fibre core, divides, as shown in figure 10.
As desired or required, by suspension 80 with fibrillating fibre, the nanofiber suspension 86 of section processes, the perhaps last nanofiber suspension of handling 88 turns back to the above-mentioned refiner stage 70 as circulation 32,90 and/100, be used for other open circuit and/or closed circuit refining, can further handle fibrous suspension.
The speed that fiber supplies to first refiner 70 depends on the specification requirement of last fibrillating fibre.This charging rate (with dried fiber) changes in about 20 to 1000lbs./hr (9-450kg/hr) usually, and the mean residence time in each refiner is between about 30 minutes to 2 hours.The number that satisfies the continuous refining machine of such manufacturing speed can change from 2 to 10.The refiner temperature inside remains on below the 175OF (80 degrees centigrade) usually.
The feature of the nanofiber 84 of this processing adopts the Canadian Standard Freeness rate representation of fibre blend, and passes through measuring method.Usually, the fibrillating fibre 80 of beginning has the CSF speed of about 50-0.Though the last CSF speed of the nanofiber of handling 84 still is 0, the optical measurement value illustrates, and under the high shear force and/or homogenising effect in closing the stream refining, fibrillation separates from fibre core and fibre core is fractured into nanofiber.
Example 1
CSF is that the mud of 0 fibrillating fibre is fed into closing in the low shear refiner of stream of Fig. 3 and 4 shown types.This fibrillating fibre mud is calculated by weight has about 1.5% solids content concn.Under the rotating speed of about 500rev/min, minimum 30 to 45 minutes of fibrillating fibre mud conditioning.At nanofiber after separating from fibre core, this core part cracking is nanofiber, and this mud is fed into closing in the stream high shear refiner of Fig. 5 and 6 shown types.In this stage, untreated pristine fibre core by refining to produce more nanofiber.Under the rotating speed of about 3600rev/min, fiber pulp was handled minimum 1 hour.The mud of this generation comprises under about 50-500nm scope and the approximately nanofiber of the fibre length of 0.5-3mm of diameter.
Example 2
Approximately the 0.5wt.% solids content and and CSF be in the upstream chamber of 0 the fibrillating fibre mud homogenising device that is fed into type shown in Figure 7.Nanofiber in this stage still mainly is connected on the core fibre.This charging rate remains on 1 liter/min (2lbs/hr of dried fiber).20, the presser unit of 000psi (140MPa) forces fiber pulp to pass through nozzle.This nozzle diameter remains on 0.2 millimeter.Fiber pulp enters in the reactor of absorptive unit, and it is used for absorbing kinetic energy.The end of the absorptive unit that the mud that produces is assembled.Then, this mud turns back in the upstream chamber, with reprocessing, is converted into nanofiber up to nanofiber separation and core fibre.
Thereby, the invention provides a kind of method and system of making the nano-scale fiber of improvement, this nanofiber does not have bigger fibre core substantially and is blended in wherein, and has bigger uniformity and flowability.The length of the diameter of the about 500-5000nm of this fibre core and about 0.1-6mm, and this Nanometer core has the length of diameter and the about 0.1-6mm of about 50-500nm.The present invention is also high, and the nano-scale fiber is made on efficient and productivity ratio ground, and causes the volume and the output that improve.The nanofiber applications that this nanofiber can be used for filtering or other are known.
Though the present invention has carried out special description in conjunction with particularly preferred embodiment, clearly according to foregoing description, many alternatives, modifications and variations are obvious to those skilled in the art.Therefore, additional claim is thought and will be comprised any such alternative, modifications and variations, and they fall within true scope of the present invention and the spirit.Therefore, the present invention has been described.
Claims (21)
1. method of making nanofiber (nanofibers), it comprises:
Prepare the suspension of fiber;
Shear this fiber of refining to produce fibrillating fibre; And close stream refining or homogenising fibrillating fibre subsequently, from fibrillating fibre, to isolate nanofiber.
2. the method for claim 1 also comprises and separate the nanofiber that this has separated substantially from remaining fibrillating fibre or core fibre.
3. the method for claim 1, wherein this closes the stream refining or the homogenising process additionally produces nanofiber from fibre core.
4. the method for claim 1, wherein closing the stream refining process carries out with first shear rate at first, and implement from fibrillating fibre, residual fiber core, to separate nanofiber with the second higher shear rate subsequently, and from this fibre core, produce other nanofiber.
5. the method for claim 1, wherein the fiber in suspension is sheared refining process and is produced the fibre core with attached nanofibers, and wherein closes the stream refining or the homogenising process is separated nanofiber from fibre core.
6. the method for claim 1, wherein to close the stream refining be to shear, crushing, pat and the cutting fibrillating fibre for fibrillating fibre this.
7. the method for claim 1, wherein fibrous suspension flows to closed circuit refining process or homogenising process from shearing refining process continuously.
8. the method for claim 1 also comprises removing from fibrous suspension and is shearing refining or closing the heat that stream produced between refining period.
9. the method for claim 1, wherein this fibrous suspension will be continuously and in series from shear that refining process flow to and by subsequently close the stream refining process, and comprise that controlling fiber suspension is refined to the flowing velocity of closing the stream refining from shearing.
10. the method for claim 1, wherein between the tooth that moves each other, close the stream refining process by enforcement by fibrous suspension, implement sufficient shearing force in the fiber of the tooth that separates in fibrous suspension, from fibrillating fibre, separating nanofiber, and from fibre core, optionally produce other nanofiber.
11. the method for claim 1, wherein the homogenising process can be implemented by following process, pass through the hole of a certain size by the fibrous suspension that fibrous suspension is pressurizeed and will pressurize, and on the fiber in fibrous suspension under the pressure, implement enough shearing forces, from fibrillating fibre, separating nanofiber, and from fibre core, optionally produce other nanofiber.
12. a method of making nanofiber, it comprises: preparation comprises the suspension of the fibrillating fibre of fibre core, and wherein this fibre core has the nanofiber that adheres to; With
Under first shear rate, close stream refining or homogenising fibrillating fibre at first, from fibre core, separate nanofiber with the second higher shear rate subsequently, and from this fibre core, produce other nanofiber.
13. method as claimed in claim 12, wherein to close the stream refining be to shear, crushing, pat and the cutting fibrillating fibre for fibrillating fibre this.
14. method as claimed in claim 12, wherein this fibrous suspension flow to second rotor that moves with second shear rate from the first rotor with the operation of first shear rate.
15. method as claimed in claim 12, wherein this fibrous suspension flow to second rotor that moves with second shear rate continuously from the first rotor with the operation of first shear rate.
16. method as claimed in claim 12, wherein this fibrous suspension flow to second rotor that moves with second shear rate continuously and in series from the first rotor with the operation of first shear rate, and comprises the flow rate of controlling fiber suspension.
17. method as claimed in claim 12 also comprises removing from fibrous suspension and is closing the heat that stream produced between refining period.
18. method as claimed in claim 12, between a pair of tooth that moves each other, close the stream refining process by fibrous suspension by enforcement, implement sufficient shearing force on the fiber of the tooth that separates in fibrous suspension, from fibrillating fibre, separating nanofiber, and from fibre core, produce other nanofiber.
19. method as claimed in claim 12, wherein the homogenising process can be implemented by following process, pass through the hole of a certain size by the fibrous suspension that fibrous suspension is pressurizeed and will pressurize, and on the fiber in fibrous suspension under the pressure, implement enough shearing forces, from fibrillating fibre, separating nanofiber, and from fibre core, produce other nanofiber.
20. fibre composition, it comprises the mixture of fibre core and the nanofiber that separates from fibre core, this fibre core has the length of diameter and the about 0.1-6mm of about 500-5000nm, and this nanofiber has the length of diameter and the about 0.1-6mm of about 50-500nm.
21. a fibre composition, it comprises the nanofiber that does not have fibre core substantially, and this nanofiber has the length of diameter and the about 0.1-6mm of about 50-500nm.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US84206906P | 2006-08-31 | 2006-08-31 | |
| US60/842,069 | 2006-08-31 | ||
| US11/694,087 | 2007-03-30 |
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| CN101512051A true CN101512051A (en) | 2009-08-19 |
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| CNA2007800321528A Pending CN101512051A (en) | 2006-08-31 | 2007-05-29 | Process for producing nanofibers |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102720087A (en) * | 2012-06-15 | 2012-10-10 | 金东纸业（江苏）股份有限公司 | Size preparation method, size and paper made of size |
| CN104894668A (en) * | 2010-05-11 | 2015-09-09 | Fp创新研究中心 | Cellulose nanofilaments and method to produce same |
| CN105705686A (en) * | 2013-03-06 | 2016-06-22 | 海克私人有限公司 | An apparatus for producing nano-bodies |
| CN108350655A (en) * | 2015-08-27 | 2018-07-31 | 斯道拉恩索公司 | The method and apparatus for being used to prepare fibrillation cellulose fibre |
| CN108474175A (en) * | 2015-12-04 | 2018-08-31 | 赛佩荷兰服务有限公司 | The method for reducing the total energy consumption in nano-cellulose manufacture |
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2007
- 2007-05-29 CN CNA2007800321528A patent/CN101512051A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104894668A (en) * | 2010-05-11 | 2015-09-09 | Fp创新研究中心 | Cellulose nanofilaments and method to produce same |
| CN102720087A (en) * | 2012-06-15 | 2012-10-10 | 金东纸业（江苏）股份有限公司 | Size preparation method, size and paper made of size |
| CN102720087B (en) * | 2012-06-15 | 2016-05-11 | 金东纸业（江苏）股份有限公司 | The preparation method of slurry, slurry and the paper being made by it |
| CN105705686A (en) * | 2013-03-06 | 2016-06-22 | 海克私人有限公司 | An apparatus for producing nano-bodies |
| CN105705686B (en) * | 2013-03-06 | 2018-01-02 | 海克私人有限公司 | Equipment for making nanometer body |
| CN108350655A (en) * | 2015-08-27 | 2018-07-31 | 斯道拉恩索公司 | The method and apparatus for being used to prepare fibrillation cellulose fibre |
| CN108350655B (en) * | 2015-08-27 | 2020-07-17 | 斯道拉恩索公司 | Method and apparatus for producing microfibrillated cellulose fibers |
| CN108474175A (en) * | 2015-12-04 | 2018-08-31 | 赛佩荷兰服务有限公司 | The method for reducing the total energy consumption in nano-cellulose manufacture |
| CN108474175B (en) * | 2015-12-04 | 2020-08-11 | 赛佩荷兰服务有限公司 | Method for reducing total energy consumption in nanocellulose production |
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