CN107328780A - A kind of method of testing of fiber fibrillation - Google Patents
A kind of method of testing of fiber fibrillation Download PDFInfo
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- CN107328780A CN107328780A CN201710596227.0A CN201710596227A CN107328780A CN 107328780 A CN107328780 A CN 107328780A CN 201710596227 A CN201710596227 A CN 201710596227A CN 107328780 A CN107328780 A CN 107328780A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
- G01N2021/8444—Fibrous material
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Abstract
The present invention relates to a kind of method of testing of fiber fibrillation, fibre bundle is handled using sonic oscillation method, and test original fiber degree, the average value that original fiber degree is fiber fibrillation index F in fibre bundle, the point that plurality of fibers is fixed together on fibre bundle is collection spot, the minimum length of segment of fiber is respectively a and b between the two ends of fibre bundle and collection spot, corresponding maximum length is respectively c and d, (c a)/a≤10% and (d b)/b≤10%, the length of the minimum segment of fiber of length is the 0.45~0.55 of the root fibre length between the termination of fibre bundle and collection spot.Test result shows, the fibrillation situation of every fiber is than more uniform in randomly selected 50 fibers, far above the level of prior art, method of testing of the invention can more accurately characterize fiber fibrillation degree, have the advantages that easy to operate, efficiency high, test error are small.
Description
Technical field
The invention belongs to fiber check and measure field, it is related to a kind of method of testing of fiber fibrillation.
Background technology
The fibrillation process of fiber refers to the process of that fiber surface divides a diameter of 1 μm~4 μm of tiny microfibre,
The mechanical property such as the original fiber degree of fiber and the stability of fiber, gas permeability and tension failure is closely related, is researcher
Study fibre property essential technical indicator, therefore, in recent years, for fiber fibrillation degree method of testing by
Gradually turn into the study hotspot of researcher.
In order to obtain the technical indicator of accurate fiber fibrillation degree, fibrillation journey of the researcher for fiber
The method of testing of degree has done substantial amounts of research.Such as document (A.Peguy and P.Gatenholm.Improvement of
adhesion between polyethylene and regenerated cellulose fibers by surface
Fibrillation researcher immerses a small amount of chopped fiber of 20mm length in distilled water in), after machinery concussion 9h, with aobvious
Fibril quantity and amount of crimp produced by micro mirror detection observation fiber, and reference standard scale is graded so that it is determined that fibre
Tie up original fiber degree；Document (Relationships between fibrillation behavior of lyocell
Fibers and their physical properties) in fiber is then immersed into Na2CO3The aqueous solution, at room temperature with 120 turns/
Min speed rocks 30min, takes out fiber and is washed and dried, with the original fiber degree of micro- sem observation sample；Document
(Physical Properties and Fibrillation Tendency of Regenerated Cellulose Fiber
Dry Jet-Wet Spun from High-Molecular Weight Cotton Linter Pulp/NMMO
Solution) in using by fiber immersion NaOH solution tested；Document (Structural characterization
and properties of Lyocell fibers after fibrillation and enzymatic
Defibrillation finishing treatments) in then handle chopped fiber with shaking the method that is combined using ball milling,
It is set to produce fibrillation and be tested；Document (Contribution to the Judgment of Fibrillability
Of Cellulosic Fibers) in by machinery rotation method test Lyocell fiber the frequency table of resistance to wet abrasion levy it
Original fiber degree；But testing process is complicated in above-mentioned test method and test process in fiber fibrillation treatment conditions it is not easily-controllable
System, is unfavorable for promoting the use of on a large scale.Above-mentioned measuring method is compared to, sonic oscillation method has equipment simple, fine because of it
The advantages of Wesy measures less, treatment conditions are easily controllable, it has also become researcher studies the important hair of fiber fibrillation measuring method
Direction is opened up, but the sonic oscillation method of original fiber degree using to(for) fiber is measured, and often freely disperses individual fibers
In treatment fluid, when carrying out ultrasonic oscillation, ultrasonic wave can decay along (radial radiation) intensity, ultimately result between Different Individual
The original fiber degree of fiber there is larger difference, the overall homogenization degree of fiber is smaller, therefore, the data meeting finally measured
There is a certain degree of error.
Therefore, study a kind of homogenization degree that can make interindividual fiber improve and easy to operate, efficiency high,
The method of testing of the small fiber fibrillation of test error is significant.
The content of the invention
The invention aims to overcome above-mentioned defect of the prior art to make between Different Individual there is provided one kind
Fiber homogenization degree improve and the small fiber fibrillation of easy to operate, efficiency high, test error method of testing.
In order to achieve the above object, the technical solution adopted by the present invention is：
A kind of method of testing of fiber fibrillation, is handled fibre bundle, and test fibrillation using sonic oscillation method
Fiber in degree, the fibre bundle is cellulose fibre, azelon, the regeneration composite fibre of containing cellulose, containing protein
Regeneration composite fibre, aramid fiber or polybenzoxazole fibers, method of testing of the invention be equally applicable to other easily produce it is former
The fiber of fibrillation, the average value that the original fiber degree is fiber fibrillation index F in fibre bundle；
The point that plurality of fibers is fixed together on the fibre bundle is collection spot, fine between the two ends of fibre bundle and collection spot
The minimum length of dimension section is respectively a and b, and corresponding maximum length is respectively c and d, and (c-a)/a≤10% and (d-b)/b≤
10%, between the termination of fibre bundle and collection spot the length of the minimum segment of fiber of length for the root fibre length 0.45~
0.55；
Fibre bundle by the way that plurality of fibers is arranged parallel to each other after fixing point aggregation bunchy and to two is chosen on fiber
Obtain, can also be consolidated the middle part of every fiber by the way that plurality of fibers is trimmed to after certain length range after the trimming of end
Aggregation bunchy together is scheduled on to obtain；
Accounting of the quantity of the 50 homogeneous fibrillation of fiber randomly selected in the fibre bundle in total radical 50 is more than
90%, the quantity of the homogeneous fibrillation of 50 fibers for fibrillation index F in 50 fibers fiber of the difference within 0.2
Radical.The quantity that 50 obtained using the method for testing of prior art dissipate fine homogeneous fibrillation is less than the 70% of total amount.
The fibrillation situation of every fiber in synnema of the present invention is than more uniform, and synnema is fixed due to centre, and two ends are to consolidating
Segment of fiber between fixed point can not be freely dispersed in water, therefore be essentially identical by the action intensity of ultrasonic wave, when every
The fibrillation situation of root fiber all than it is more uniform when, the original fiber degree characterized by its average value can more accurately reflect this kind of fiber
Fibrillation characteristic, reduce due to the larger error caused of different fiber fibrillation difference, and prior art due to be dissipate fibre,
In ultrasonic wave, each position has, and ultrasonic wave is unlikely to be isotropism and (radial radiation) intensity can decay, therefore not
The fibrillation situation of fiber can be performed well in reflecting, while prior art typically takes fiber 10 or so, fiber number is few, point
Dissipate position difference larger, it is different by ultrasonication intensity, therefore uniformity is poor.
It is used as preferred technical scheme：
A kind of method of testing of fiber fibrillation as described above, the cellulose fibre is cotton fiber, flaxen fiber or again
Raw cellulose fibre, the azelon is wool fiber, silk fiber or regenerated protein, the regenerated celulose fibre
For Lyocell fiber, viscose rayon or Model fibers etc., the regenerated protein is fibroin fiber etc., and one is only listed here
The fibrous material commonly used a bit, protection scope of the present invention includes but is not limited to cited material.
A kind of method of testing of fiber fibrillation as described above, it is to knot, tie up that the bunchy mode of the fibre bundle, which is,
Or bonding.
In a kind of method of testing of fiber fibrillation as described above, the fibre bundle length of every fiber for 10~
40mm, the length of fiber is oversize easily to tangle, too short bad operation.
A kind of method of testing of fiber fibrillation as described above, the specific method of the processing is：First by fibre bundle
Dispersion liquid is obtained in immersion deionized water, bath raio (fiber/deionized water) is 0.05~0.25mg/mL, then puts dispersion liquid
In 0~5 DEG C of ice-water bath, and it is ultrasonically treated to dispersion liquid progress, fibre bundle is finally taken out, surface moisture is removed.
A kind of method of testing of fiber fibrillation as described above, it is described it is ultrasonically treated use for the ultrasounds of Bilon 500
Wave pressure electric tachometer indicator ultrasonoscope, the distance between ultrasonic probe and dispersion liquid bottom are 5~20mm, ultrasonic power is 300~
600W, sonication treatment time is 10~50min.
A kind of method of testing of fiber fibrillation as described above, the distance between the ultrasonic probe and dispersion liquid bottom
For 10mm, ultrasonic power is 500W, and sonication treatment time is 30min.This technical scheme is best-of-breed technology scheme of the invention,
The original fiber degree between the most clearly fibrillation design sketch, fiber sample can be now obtained to be easiest to distinguish identification.
A kind of method of testing of fiber fibrillation as described above, the test original fiber degree uses microscope sight
Examine method.
A kind of method of testing of fiber fibrillation as described above, the microscope observation concrete operations are：From processing
The fiber sample of the multiple 2~5mm length of clip, is placed on clean slide in wet fiber beam afterwards, and glycerine is added dropwise and causes fiber
Sample dispersion, covers slide, is placed on the micro- Microscopic observation with digital camera head annex, regulation multiplication factor is to clearly
Taken pictures afterwards, count the radical and length for the fibril that each fiber sample is produced, calculate fibrillation index F, take its average value.
A kind of method of testing of fiber fibrillation as described above, the calculation formula of the fibrillation index F is as follows：
In formula, liFor i-th fibril length, L is the length of fiber sample.
Beneficial effect：
(1) a kind of method of testing of fiber fibrillation of the invention, easy to operate, the fibril of ultrasonically treated rear every fiber
Change degree is more homogeneous, can more accurately and efficiently characterize the original fiber degree of fiber, reduces error, is pushed away with fabulous
Wide value.
(2) method of testing of a kind of fiber fibrillation of the invention, the fibrillation effect of the fiber finally given can be aobvious
Clearly recognized under micro mirror, be conducive to clearly distinguishing the species of fiber.
Brief description of the drawings
Fig. 1 is fibre bundle schematic diagram of the invention；
Fig. 2 is supersonic oscillations schematic device of the invention.
Embodiment
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this hair
Bright rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, art technology
Personnel can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Fixed scope.
Embodiment 1
A kind of method of testing of cotton fiber fibrillation, step is as follows：
(1) fibre bundle is prepared, the bunchy mode of fibre bundle is is to knot, and the weight of fibre bundle is 1.1mg, as shown in figure 1,
The point that many cotton fibers are fixed together on fibre bundle is collection spot, the minimum of segment of fiber between the two ends of fibre bundle and collection spot
Length is respectively a and b, and corresponding maximum length is respectively c and d, and (c-a)/a is that 0% and (d-b)/b is 0%, the end of fibre bundle
The length of the minimum segment of fiber of length is the length of every fiber in the 0.5 of the root fibre length, fibre bundle between head and collection spot
Spend for 20mm；
(2) dispersion liquid, wherein bath raio (fiber/deionized water) are obtained as shown in Fig. 2 fibre bundle is immersed in deionized water
For 0.11mg/mL, then dispersion liquid is placed in 0 DEG C of ice-water bath, and utilizes the ultrasound piezoelectric oscillator ultrasonic waves of Bilon 500
Instrument is ultrasonically treated to dispersion liquid progress, and wherein the distance between ultrasonic probe and dispersion liquid bottom are 10mm, and ultrasonic power is
300W, sonication treatment time is 10min, finally takes out fibre bundle, removes surface moisture；
(3) from wet fiber beam 50 2mm length of clip fiber sample, be placed on clean slide, be added dropwise glycerine make
Obtain fiber sample to disperse, cover slide, be placed on the micro- Microscopic observation with digital camera head annex, adjust multiplication factor
To the clear rear radical and length taken pictures, count the fibril that each fiber sample is produced, fibrillation index F is calculated, it is taken
Average value, it is 4.0 that calculating, which obtains its average value,.
Test result shows that fibrillation index F difference is within 0.2 in the fiber of 50 randomly selected in fibre bundle piece
Accounting of the radical of fiber in total radical 50 is 93%.
Comparative example 1
A kind of method of testing of cotton fiber fibrillation, basic step be the same as Example 1, difference is that cotton fiber does not have
Assemble bunchy, be when ultrasonically treated random dispersion in deionized water, test result shows, is randomly selected in fibre bundle
Accounting of the radical of fiber of the fibrillation index F difference within 0.2 in total radical 50 is 60% in 50 fibers.Will be real
Example 1 is applied to contrast with comparative example 1 as can be seen that the application substitutes the staple in bulk in conventional ultrasound succusion, fiber using fibre bundle
Overall homogenization degree is significantly improved, and the original fiber degree between individual fibers is roughly the same, so that finally measure 50
Fibrillation index F value is all closer between root fiber, herein under the premise of, the final average value using fibrillation index is come table
The original fiber degree of fiber is levied just closer to truth, therefore, the present invention can it is more objective, characterize fiber exactly
Original fiber degree.
Embodiment 2
A kind of method of testing of flaxen fiber fibrillation, step is as follows：
(1) fibre bundle is prepared, the bunchy mode of fibre bundle is is to knot, and the weight of fibre bundle is many on 1.8mg, fibre bundle
The point that root flaxen fiber is fixed together is collection spot, and the minimum length of segment of fiber is respectively between the two ends of fibre bundle and collection spot
A and b, corresponding maximum length is respectively c and d, and (c-a)/a is that 10% and (d-b)/b is 10%, the termination of fibre bundle and boundling
Between point the length of the minimum segment of fiber of length be the length of every fiber in the 0.55 of the root fibre length, fibre bundle for 10~
40mm；
(2) fibre bundle is immersed and dispersion liquid is obtained in deionized water, wherein bath raio (fiber/deionized water) is 0.18mg/
Dispersion liquid, is then placed in 0 DEG C of ice-water bath by mL, and using the ultrasound piezoelectric oscillator ultrasonoscopes of Bilon 500 to scattered
Liquid progress is ultrasonically treated, and wherein the distance between ultrasonic probe and dispersion liquid bottom are 5mm, and ultrasonic power is 300W, ultrasound
Processing time is 10min, finally takes out fibre bundle, removes surface moisture；
(3) from wet fiber beam 50 2mm length of clip fiber sample, be placed on clean slide, be added dropwise glycerine make
Obtain fiber sample to disperse, cover slide, be placed on the micro- Microscopic observation with digital camera head annex, adjust multiplication factor
To the clear rear radical and length taken pictures, count the fibril that each fiber sample is produced, fibrillation index F is calculated, it is taken
Average value, it is 1.3 that calculating, which obtains its average value,.
Test result shows that fibrillation index F difference is within 0.2 in the fiber of 50 randomly selected in fibre bundle piece
Accounting of the radical of fiber in total radical 50 is 90.5%.
Embodiment 3
A kind of method of testing of graphene/cellulose composite fiber fibrillation, be the same as Example 2, final calculate obtains fibril
The difference that the average value for changing index F is fibrillation index F in 50 fibers randomly selected in 0.4, fibre bundle is within 0.2
Accounting of the radical of fiber in total radical 50 is 93.0%.
Embodiment 4
A kind of TiO2The method of testing of/cellulose composite fiber fibrillation, be the same as Example 2, final calculate obtains fibrillation
Index F average value is 0.3, fibre of the fibrillation index F difference within 0.2 in 50 fibers randomly selected in fibre bundle
Accounting of the radical of dimension in total radical 50 is 95.0%.
Embodiment 5
A kind of method of testing of wool fiber fibrillation, step is as follows：
(1) fibre bundle is prepared, the bunchy mode of fibre bundle is is to tie up, and the weight of fibre bundle is many on 2.3mg, fibre bundle
The point that root wool fiber is fixed together is collection spot, and the minimum length of segment of fiber is distinguished between the two ends of fibre bundle and collection spot
For a and b, corresponding maximum length is respectively c and d, and (c-a)/a is that 8% and (d-b)/b is 6%, the termination of fibre bundle and boundling
Between point the length of the minimum segment of fiber of length be the length of every fiber in the 0.45 of the root fibre length, fibre bundle for 10~
40mm；
(2) fibre bundle is immersed and dispersion liquid is obtained in deionized water, wherein bath raio (fiber/deionized water) is 0.25mg/
Dispersion liquid, is then placed in 5 DEG C of ice-water bath by mL, and using the ultrasound piezoelectric oscillator ultrasonoscopes of Bilon 500 to scattered
Liquid progress is ultrasonically treated, and wherein the distance between ultrasonic probe and dispersion liquid bottom are 10mm, and ultrasonic power is 500W, ultrasound
Processing time is 30min, finally takes out fibre bundle, removes surface moisture；
(3) from wet fiber beam 50 3mm length of clip fiber sample, be placed on clean slide, be added dropwise glycerine make
Obtain fiber sample to disperse, cover slide, be placed on the micro- Microscopic observation with digital camera head annex, adjust multiplication factor
To the clear rear radical and length taken pictures, count the fibril that each fiber sample is produced, fibrillation index F is calculated, it is taken
Average value, it is 0.9 that calculating, which obtains its average value,.
Test result shows that fibrillation index F difference is within 0.2 in the fiber of 50 randomly selected in fibre bundle piece
Accounting of the radical of fiber in total radical 50 is 98%.
Embodiment 6
A kind of method of testing of protein/cellulose composite fiber fibrillation, be the same as Example 5, final calculate obtains fibril
The difference that the average value for changing index F is fibrillation index F in 50 fibers randomly selected in 0.6, fibre bundle is within 0.2
Accounting of the radical of fiber in total radical 50 is 90%.
Embodiment 7
A kind of method of testing of milk protein composite fibre fibrillation, be the same as Example 5, final calculate obtains fibrillation index
F average value is 1.2, fiber of the fibrillation index F difference within 0.2 in 50 fibers randomly selected in fibre bundle
Accounting of the radical in total radical 50 is 93%.
Embodiment 8
A kind of method of testing of silk fiber fibrillation, step is as follows：
(1) fibre bundle is prepared, the bunchy mode of fibre bundle is is bonding, and the weight of fibre bundle is many on 1.8mg, fibre bundle
The point that root silk fiber is fixed together is collection spot, and the minimum length of segment of fiber is distinguished between the two ends of fibre bundle and collection spot
For a and b, corresponding maximum length is respectively c and d, and (c-a)/a is that 5% and (d-b)/b is 7%, the termination of fibre bundle and boundling
Between point the length of the minimum segment of fiber of length be the length of every fiber in the 0.5 of the root fibre length, fibre bundle for 10~
40mm；
(2) fibre bundle is immersed and dispersion liquid is obtained in deionized water, wherein bath raio (fiber/deionized water) is 0.18mg/
Dispersion liquid, is then placed in 3 DEG C of ice-water bath by mL, and using the ultrasound piezoelectric oscillator ultrasonoscopes of Bilon 500 to scattered
Liquid progress is ultrasonically treated, and wherein the distance between ultrasonic probe and dispersion liquid bottom are 8mm, and ultrasonic power is 600W, ultrasound
Processing time is 50min, finally takes out fibre bundle, removes surface moisture；
(3) from wet fiber beam 50 5mm length of clip fiber sample, be placed on clean slide, be added dropwise glycerine make
Obtain fiber sample to disperse, cover slide, be placed on the micro- Microscopic observation with digital camera head annex, adjust multiplication factor
To the clear rear radical and length taken pictures, count the fibril that each fiber sample is produced, fibrillation index F is calculated, it is taken
Average value, it is 6.0 that calculating, which obtains its average value,.
Test result shows that fibrillation index F difference is within 0.2 in the fiber of 50 randomly selected in fibre bundle piece
Accounting of the radical of fiber in total radical 50 is 97%.
Embodiment 9
A kind of method of testing of aramid fiber fibrillation, be the same as Example 8, final calculate obtains fibrillation index F average value and is
6.7, the radical of fiber of the fibrillation index F difference within 0.2 is in total root in 50 fibers randomly selected in fibre bundle
Accounting in number 50 is 94%.
Embodiment 10
A kind of method of testing of Lyocell fiber fibrillation, step is as follows：
(1) fibre bundle is prepared, the bunchy mode of fibre bundle is is bonding, and the weight of fibre bundle is many on 1.0mg, fibre bundle
The point that root Lyocell fiber is fixed together is collection spot, the minimum length of segment of fiber between the two ends of fibre bundle and collection spot
Respectively a and b, corresponding maximum length is respectively c and d, and (c-a)/a is that 0% and (d-b)/b is 0%, the termination of fibre bundle with
The length of the minimum segment of fiber of length is that the length of every fiber in the 0.5 of the root fibre length, fibre bundle is between collection spot
20mm；
(2) fibre bundle is immersed and dispersion liquid is obtained in deionized water, wherein bath raio (fiber/deionized water) is 0.10mg/
Dispersion liquid, is then placed in 2 DEG C of ice-water bath by mL, and using the ultrasound piezoelectric oscillator ultrasonoscopes of Bilon 500 to scattered
Liquid progress is ultrasonically treated, and wherein the distance between ultrasonic probe and dispersion liquid bottom are 12mm, and ultrasonic power is 500W, ultrasound
Processing time is 30min, finally takes out fibre bundle, removes surface moisture；
(3) from wet fiber beam 50 3mm length of clip fiber sample, be placed on clean slide, be added dropwise glycerine make
Obtain fiber sample to disperse, cover slide, be placed on the micro- Microscopic observation with digital camera head annex, adjust multiplication factor
To the clear rear radical and length taken pictures, count the fibril that each fiber sample is produced, fibrillation index F is calculated, it is taken
Average value, it is 15.0 that calculating, which obtains its average value,.
Test result shows that fibrillation index F difference is within 0.2 in the fiber of 50 randomly selected in fibre bundle piece
Accounting of the radical of fiber in total radical 50 is 96%.
Embodiment 11
A kind of method of testing of polybenzoxazole fibers fibrillation, be the same as Example 10, final calculate obtains fibrillation index F
Average value be 8.0, fiber of the fibrillation index F difference within 0.2 in 50 fibers randomly selected in fibre bundle
Accounting of the radical in total radical 50 is 91%.
Embodiment 12
A kind of method of testing of viscose rayon fibrillation, step is as follows：
(1) fibre bundle is prepared, the bunchy mode of fibre bundle is is to knot, and the weight of fibre bundle is many on 2.0mg, fibre bundle
The point that root viscose rayon is fixed together is collection spot, and the minimum length of segment of fiber is distinguished between the two ends of fibre bundle and collection spot
For a and b, corresponding maximum length is respectively c and d, and (c-a)/a is that 0% and (d-b)/b is 1%, the termination of fibre bundle and boundling
Between point the length of the minimum segment of fiber of length be the length of every fiber in the 0.52 of the root fibre length, fibre bundle for 10~
40mm；
(2) fibre bundle is immersed and dispersion liquid is obtained in deionized water, wherein bath raio (fiber/deionized water) is 0.20mg/
Dispersion liquid, is then placed in 3 DEG C of ice-water bath by mL, and using the ultrasound piezoelectric oscillator ultrasonoscopes of Bilon 500 to scattered
Liquid progress is ultrasonically treated, and wherein the distance between ultrasonic probe and dispersion liquid bottom are 13mm, and ultrasonic power is 450W, ultrasound
Processing time is 30min, finally takes out fibre bundle, removes surface moisture；
(3) from wet fiber beam 50 4mm length of clip fiber sample, be placed on clean slide, be added dropwise glycerine make
Obtain fiber sample to disperse, cover slide, be placed on the micro- Microscopic observation with digital camera head annex, adjust multiplication factor
To the clear rear radical and length taken pictures, count the fibril that each fiber sample is produced, fibrillation index F is calculated, it is taken
Average value, it is 0.1 that calculating, which obtains its average value,.
Test result shows that fibrillation index F difference is within 0.2 in the fiber of 50 randomly selected in fibre bundle piece
Accounting of the radical of fiber in total radical 50 is 95%.
Embodiment 13
A kind of method of testing of Model fiber fibrillations, step is as follows：
(1) fibre bundle is prepared, the bunchy mode of fibre bundle is is bonding, and the weight of fibre bundle is many on 1.8mg, fibre bundle
The point that root Model fibers are fixed together is collection spot, the minimum length point of segment of fiber between the two ends of fibre bundle and collection spot
Not Wei a and b, corresponding maximum length is respectively c and d, and (c-a)/a is that 3% and (d-b)/b is 2%, the termination of fibre bundle and collection
The length of the minimum segment of fiber of length is that the length of every fiber in the 0.53 of the root fibre length, fibre bundle is 10 between spot
~40mm；
(2) fibre bundle is immersed and dispersion liquid is obtained in deionized water, wherein bath raio (fiber/deionized water) is 0.18mg/
Dispersion liquid, is then placed in 4 DEG C of ice-water bath by mL, and using the ultrasound piezoelectric oscillator ultrasonoscopes of Bilon 500 to scattered
Liquid progress is ultrasonically treated, and wherein the distance between ultrasonic probe and dispersion liquid bottom are 15mm, and ultrasonic power is 400W, ultrasound
Processing time is 20min, finally takes out fibre bundle, removes surface moisture；
(3) from wet fiber beam 50 5mm length of clip fiber sample, be placed on clean slide, be added dropwise glycerine make
Obtain fiber sample to disperse, cover slide, be placed on the micro- Microscopic observation with digital camera head annex, adjust multiplication factor
To the clear rear radical and length taken pictures, count the fibril that each fiber sample is produced, fibrillation index F is calculated, it is taken
Average value, it is 0.2 that calculating, which obtains its average value,.
Test result shows that fibrillation index F difference is within 0.2 in the fiber of 50 randomly selected in fibre bundle piece
Accounting of the radical of fiber in total radical 50 is 90%.
Embodiment 14
A kind of method of testing of fibroin fiber fibrillation, step is as follows：
(1) fibre bundle is prepared, the bunchy mode of fibre bundle is is bonding, and the weight of fibre bundle is many on 2.2mg, fibre bundle
The point that root fibroin fiber is fixed together is collection spot, and the minimum length of segment of fiber is distinguished between the two ends of fibre bundle and collection spot
For a and b, corresponding maximum length is respectively c and d, and (c-a)/a is that 5% and (d-b)/b is 6%, the termination of fibre bundle and boundling
Between point the length of the minimum segment of fiber of length be the length of every fiber in the 0.54 of the root fibre length, fibre bundle for 10~
40mm；
(2) fibre bundle is immersed and dispersion liquid is obtained in deionized water, wherein bath raio (fiber/deionized water) is 0.22mg/
Dispersion liquid, is then placed in 3 DEG C of ice-water bath by mL, and using the ultrasound piezoelectric oscillator ultrasonoscopes of Bilon 500 to scattered
Liquid progress is ultrasonically treated, and wherein the distance between ultrasonic probe and dispersion liquid bottom are 18mm, and ultrasonic power is 350W, ultrasound
Processing time is 15min, finally takes out fibre bundle, removes surface moisture；
(3) from wet fiber beam 50 2mm length of clip fiber sample, be placed on clean slide, be added dropwise glycerine make
Obtain fiber sample to disperse, cover slide, be placed on the micro- Microscopic observation with digital camera head annex, adjust multiplication factor
To the clear rear radical and length taken pictures, count the fibril that each fiber sample is produced, fibrillation index F is calculated, it is taken
Average value, it is 5.0 that calculating, which obtains its average value,.
Test result shows that fibrillation index F difference is within 0.2 in the fiber of 50 randomly selected in fibre bundle piece
Accounting of the radical of fiber in total radical 50 is 92%.
Claims (10)
1. a kind of method of testing of fiber fibrillation, it is characterized in that：Fibre bundle is handled using sonic oscillation method, and tested
Fiber in original fiber degree, the fibre bundle is cellulose fibre, azelon, the regeneration composite fibre of containing cellulose, contained
Regeneration composite fibre, aramid fiber or the polybenzoxazole fibers of protein, the original fiber degree are fiber fibrillation in fibre bundle
Index F average value；
The point that plurality of fibers is fixed together on the fibre bundle is collection spot, segment of fiber between the two ends of fibre bundle and collection spot
Minimum length be respectively a and b, corresponding maximum length is respectively c and d, (c-a)/a≤10% and (d-b)/b≤10%, fine
The length for tieing up the minimum segment of fiber of length between the termination of beam and collection spot is the 0.45~0.55 of the root fibre length；
Accounting of the quantity of the 50 homogeneous fibrillation of fiber randomly selected in the fibre bundle in total radical 50 is more than 90%,
The root of fiber of the difference that the quantity of the homogeneous fibrillation of 50 fibers is fibrillation index F in 50 fibers within 0.2
Number.
2. a kind of method of testing of fiber fibrillation according to claim 1, it is characterised in that the cellulose fibre is
Cotton fiber, flaxen fiber or regenerated celulose fibre, the azelon are wool fiber, silk fiber or regenerated protein.
3. a kind of method of testing of fiber fibrillation according to claim 1, it is characterised in that the bunchy of the fibre bundle
It is to knot, tie up or bond that mode, which is,.
4. the method for testing of a kind of fiber fibrillation according to claim 1, it is characterised in that every in the fibre bundle
The length of fiber is 10~40mm.
5. a kind of method of testing of fiber fibrillation according to claim 4, it is characterised in that the specific side of the processing
Method is：Fibre bundle is immersed first dispersion liquid is obtained in deionized water, bath raio is 0.05~0.25mg/mL, then by dispersion liquid
In the ice-water bath for being placed in 0~5 DEG C, and it is ultrasonically treated to dispersion liquid progress, fibre bundle is finally taken out, surface moisture is removed.
6. a kind of method of testing of fiber fibrillation according to claim 5, it is characterised in that the ultrasonically treated use
For the ultrasound piezoelectric oscillator ultrasonoscopes of Bilon 500, the distance between ultrasonic probe and dispersion liquid bottom are 5~20mm,
Ultrasonic power is 300~600W, and sonication treatment time is 10~50min.
7. the method for testing of a kind of fiber fibrillation according to claim 6, it is characterised in that the ultrasonic probe is with dividing
The distance between dispersion liquid bottom is 10mm, and ultrasonic power is 500W, and sonication treatment time is 30min.
8. a kind of method of testing of fiber fibrillation according to claim 1, it is characterised in that the test fibrillation journey
Degree uses microscope observation.
9. a kind of method of testing of fiber fibrillation according to claim 8, it is characterised in that the microscope observation
Concrete operations are：The fiber sample of the multiple 2~5mm length of clip, is placed on clean slide from the wet fiber beam after processing,
Glycerine, which is added dropwise, causes fiber sample to disperse, and covers slide, is placed on the micro- Microscopic observation with digital camera head annex, adjusts
Section multiplication factor calculates fibrillation to the clear rear radical and length taken pictures, count the fibril that each fiber sample is produced
Index F, takes its average value.
10. a kind of method of testing of fiber fibrillation according to claim 9, it is characterised in that the fibrillation index F
Calculation formula it is as follows：
<mrow>
<mi>F</mi>
<mo>=</mo>
<mfrac>
<mn>1</mn>
<mi>L</mi>
</mfrac>
<msubsup>
<mo>&Sigma;</mo>
<mrow>
<mi>i</mi>
<mo>=</mo>
<mn>1</mn>
</mrow>
<mi>n</mi>
</msubsup>
<msub>
<mi>l</mi>
<mi>i</mi>
</msub>
<mo>;</mo>
</mrow>
In formula, l1For i-th fibril length, L is the length of fiber sample.
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| CN113445296A (en) * | 2021-06-29 | 2021-09-28 | 泰山玻璃纤维邹城有限公司 | Device and method for detecting hollow fibers of glass fiber electronic cloth |
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2017
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Non-Patent Citations (3)
| Title |
|---|
| KYUNG YUL LIM: "Reducation of Fibrillation of Lyocell FIber with Cellulose--poly (viny alcohol ) COpolymer", 《POLYMER JOURNAL》 * |
| S. A. MORTIMER 等: "Methods for Reducing the Tendency of Lyocell Fibers to Fibrillate", 《JOURNAL OF APPLIED POLYMER SCIENCE》 * |
| 杨旭红: "Lyocell 纤维原纤化程度的评价", 《技术应用 丝绸》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113445296A (en) * | 2021-06-29 | 2021-09-28 | 泰山玻璃纤维邹城有限公司 | Device and method for detecting hollow fibers of glass fiber electronic cloth |
| CN113445296B (en) * | 2021-06-29 | 2022-11-25 | 泰山玻璃纤维邹城有限公司 | Device and method for detecting hollow fibers of glass fiber electronic cloth |
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