CN103323360B - A kind of fiber content assay method of cellulosic fibre blend product and device thereof - Google Patents
A kind of fiber content assay method of cellulosic fibre blend product and device thereof Download PDFInfo
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Abstract
The fiber content assay method of cellulosic fibre blend product and a device, wherein known containing two kinds of cellulose fibres, and at least containing the one in bamboo, fiber crops or cotton fiber; Its method: get sample after the process of element length, record total dry mass after drying; By the two kinds of fibre densities calibrated per sample, prepare density gradient separation liquid in fiber separation device, the liquid-tight degree of this density gradient separation is in sample between two kinds of fibre densities; Inserted by sample in fiber separation device, overall standing 30-60min, two kinds of fibers are separated in density gradient separation liquid; Sinking fiber leaves with density gradient separation liquid, records isolated fiber dry weight after drying; Again residual fiber is separated and aftertreatment; Finally calculate various fiber content.The method and the separation achieved the closely two kinds of fibers of performance in cellulosic fibre blend product, and separated with no damage separately by fiber in sample, therefore without the need to modified result, quantitative test accuracy rate is high.
Description
Technical field
The invention belongs to textile industry textile chemistry component quantifying analysis field, particularly relate to a kind of with the assay method of the fiber content of bamboo fibre, flaxen fiber or the cotton fiber cellulosic fibre blend product that is one of raw material and device thereof.
Background technology
Increasing of the continuous release of tencel, particularly cellulose fibre member, makes the Qualitive test of cellulosic fibre blend product and content quantitative analyze more and more difficult.Ramie bast fiber comprises flax, ramie, hemp, jute, leaf of Japanese banana fiber crops etc., and increasing kind starts to be applied in the product for civilian use; Bamboo fibre is the new type natural cellulose fibre in recent years succeeded in developing, and is also in the starting stage in the industry to the understanding of bamboo fibre, differentiates a difficult problem especially to the qualitative, quantitative of its blending product.
Bamboo fibre to be removed by physics, chemistry or the method such as biological by bamboo wood or part removes the material such as lignin, pentosan, pectin wherein, extracts the natural fiber that cellulose directly obtains.It maintains the original natural characteristic of bamboo fiber, there is the advantages such as aboundresources, dry and comfortable absorbing sweat, environmental protection.Along with people's environmental consciousness is strengthened gradually, natural bamboo fibres is pollution-free as one, environmental protection fiber, starts to be utilized gradually, but at present in textile inspection field, quantitative test for bamboo fibre rarely has document to mention, this utilization for bamboo fibre is totally unfavorable with popularization.
For the qualitative identification method of bamboo fibre, flaxen fiber, the present inventor has proposed a series of discrimination method, as the present inventor adopts fibre morphology size method to be studied the fibre length of several native cellulose fibres such as bamboo fibre, hemp, jute, ramie, flax, horizontal cross-section form in " discrimination method of several natural plant fibre " literary composition, draw and just bamboo fibre, flaxen fiber and other native cellulose fibres can be made a distinction by filament size method and fibre morphology observation.The present inventor is in " weaving bamboo fibre " LY/T1792-2008 forestry industry standard simultaneously, it is also proposed bamboo fibre qualitative identification method.Along with bamboo fibre on market, being on the increase of flaxen fiber product, in blending product, the detection of bamboo fibre, flaxen fiber content seems very necessary.
But the domestic and international quantitative judging standard about cellulose fibre is very limited at present.In the standard of cellulose fibre quantitative test, majority is the discriminating of native cellulose fibre and regenerated celulose fibre, as in textile quantitative chemical analysis: the quantitative test of viscose fiber, some CUP or Modal fibre and cotton potpourri sodium zincate method; The quantitative test of viscose fiber, some CUP, Modal fibre or Lyocell fibers and cotton potpourri formic acid zinc chloride process; The quantitative test of the potpourri formic acid zinc chloride process of viscose fiber, some CUP or Modal fibre and flax, ramie; The sulfuric acid process quantitative test of the potpourri of cellulose fibre and dacron; The assay methods such as regenerated celulose fibre and the quantitative analysis method of flax fiber blending product hydrochloric acid method.In a word, the quantitative discriminating of cellulose fibre adopts chemical dissolution method and microscope physical aspect method two kinds usually.Wherein, speed is slow, efficiency is low, accuracy rate is low for microscopic method (only having the microscope physical aspect quantitative analysis of cotton fiber/flaxen fiber at present), and can only test with flax fiber blending product for cotton; Chemical dissolution method for the quantitative discriminating of cellulose fibre and synthon, cellulose fibre and protein fibre, native cellulose fibre and regenerated celulose fibre, and can only cannot realize the fiber content quantitative test to native cellulose fibre and native cellulose fibre blending product.
Due to the cellulose fibre structure that particularly native cellulose fibre is mutual, performance difference is very little, and with regard to a kind of natural fiber, the mutual density of fiber also has certain discrete, if so can only be separated by two kinds of fibers larger to performance difference by the relative density method proposed in " textile fibres discriminating handbook " book, when tested object is performance sample closely, fiber separation thickness, the separating layer of two kinds of fibers is obscured, be separated unclear, therefore fibre density bamboo fibre closely cannot be used for, cotton, fiber separation in the blending products such as fiber crops and viscose fiber.
Summary of the invention
Fundamental purpose of the present invention is to provide a kind of with the fiber content assay method of bamboo fibre, flaxen fiber or the cotton fiber cellulosic fibre blend product that is one of raw material, and its assay method is simple and reliable.
For achieving the above object, the present invention is by the following technical solutions:
A fiber content assay method for cellulosic fibre blend product, has known containing two kinds of cellulose fibres in this blending product, and at least containing the one in bamboo fibre, flaxen fiber and cotton fiber; Its method step is as follows:
A) pre-service of removing non-fibrous material is carried out to the sample of cellulosic fibre blend product to be measured;
B) get sample after the pre-service of a 1 element length, after final drying, record its total dry mass, stand-by;
C) in fiber separation device, density gradient separation liquid is prepared by the density of the two kinds of cellulose fibres calibrated according in this sample, between the density of density two kinds of cellulose fibres in this sample of this density gradient separation liquid, and density becomes large from top to bottom gradually, and continuous distribution forms gradient; With openable separating opening bottom this fiber separation device, a filtration unit of weighing is in advance set in the below of fiber separation device separating opening;
D) after the preparation of density gradient separation liquid terminates, testing sample is inserted in fiber separation device; Overall standing 30-60min;
E) open the separating opening of fiber separation device, the first fiber sunk after leaving standstill is separated in filtration unit with density gradient separation liquid;
F) by the first fiber drying process isolated, the first fiber dry weight isolated is recorded;
G) by the second fiber separation remained in fiber separation device, dry process, record the second fiber dry weight;
H) the various fiber contents of this cellulosic fibre blend product are calculated:
In the fiber content assay method of above-mentioned cellulosic fibre blend product, the concrete preparation of described density gradient separation liquid: light, the heavy-fluid preprepared with two kinds of different densities inject fiber separation device according to the secondary Order continuous that density is descending, rate of addition 8 ~ 10mL/min, wherein, light liquid density is greater than the density of the light fiber in sample, and heavy-fluid density is less than the density of the heavy fiber in sample.
A fiber content assay method for cellulosic fibre blend product, has known containing first, second, and third totally three kinds of cellulose fibres by the descending sequence of density in this blending product, and at least containing the one in bamboo fibre, flaxen fiber and cotton fiber; Its method step is as follows:
A) pre-service of removing non-fibrous material is carried out to the sample of cellulosic fibre blend product to be measured;
B) get sample after the pre-service of two parts of 1 element lengths, after final drying, record total dry mass of every increment product, stand-by;
C) according in this sample by the density of three kinds of cellulose fibres calibrated, preparation first and second liang group density gradient separation liquid in the first and second two fiber separation devices respectively, the density of each group of density gradient separation liquid becomes large from top to bottom gradually, and continuous distribution forms gradient; Wherein: the density of first group of density gradient separation liquid is between the density of the first and second two kinds of cellulose fibres, and the density of second group of density gradient separation liquid is between second and the density of the 3 two kind of cellulose fibre;
D) two parts of testing samples are inserted respectively in the first and second two fiber separation devices, add rear respective entirety and leave standstill 30-60min;
E) separating opening bottom two fiber separation devices is opened respectively, wherein: the first fiber sunk after leaving standstill in the first fiber separation device is separated in the filtration unit of weighing be in advance preset at below the first fiber separation device separating opening with first group of density gradient separation liquid; The first of sinking after leaving standstill in the second fiber separation device is separated to second group of density gradient separation liquid in the filtration unit of weighing be in advance preset at below the second fiber separation device separating opening jointly with the second fiber, and the third fiber has remained in the second fiber separation device;
F) its dry weight is recorded in the first fiber drying process isolated in the first fiber separation device; The third fiber separation remained in the second fiber separation device, drying are processed and record its dry weight;
G) three kinds of fiber contents of this cellulosic fibre blend product are calculated:
The second fiber content (%)=the third fiber content of the first fiber content of 100%-(%+ %).
In the fiber content assay method of described cellulosic fibre blend product, the concrete preparation of described first group of density gradient separation liquid: light, the heavy-fluid preprepared with two kinds of different densities inject the first fiber separation device according to the secondary Order continuous that density is descending, rate of addition 8 ~ 10mL/min, wherein, light liquid density is greater than the density of the second fiber in sample, and heavy-fluid density is less than the density of the first fiber in sample; The concrete preparation of second group of density gradient separation liquid: light, the heavy-fluid preprepared with two kinds of different densities inject the second fiber separation device according to the secondary Order continuous that density is descending, rate of addition 8 ~ 10mL/min, wherein, light liquid density is greater than the density of the third fiber in sample, and heavy-fluid density is less than the density of the second fiber in sample.
In the fiber content assay method of above-mentioned cellulosic fibre blend product, the light or heavy-fluid of described preparation density gradient separation liquid is by two kinds of liquid mixed preparing in phenixin, methenyl choloride, methylene chloride, dimethylbenzene, first benzene and heptane; During preparation density gradient separation liquid, the feeding mouth inwall need being close to fiber separation device drips liquid, place a steel wire ring identical with spout diameter size in the feeding mouth inwall lower end with tapering of fiber separation device, make heavy-fluid, light liquid inject fiber separation device along steel wire ring successively.
In the fiber content assay method of described cellulosic fibre blend product, when described sample is the blending product of the native cellulose fibre of bast class, the process of colloid need be removed to sample: sample is immersed in mass percent concentration be 30% hydrogen peroxide and mass percent concentration glacial acetic acid 1: 1-1: 4 proportions by volume that are not less than 99.5% mixed liquor in, under the treatment temperature of 60-80 DEG C, be vibrate in 80-100r/min water-bath constant temperature oscillator at rotating speed, processing time is 24-30h, extract, suction filtration or centrifugal dehydration, natural drying, stand-by.
In the fiber content assay method of described cellulosic fibre blend product, described fiber separation device is prepended in the constant temperature water bath of 20 ± 0.5 DEG C in the preparation of density gradient separation liquid, and continue in mensuration, to keep temperature constant constant, until the fiber fractionation in sample.
Another object of the present invention is to provide a kind of fiber separation device for said determination method, and the fiber content of the cellulosic fibre blend product being one of raw material with bamboo fibre, flaxen fiber or cotton fiber by its mensuration, can carry out high-precision mensuration.
For achieving the above object, the present invention is by the following technical solutions:
A kind of fiber separation device of the fiber content assay method for above-mentioned cellulosic fibre blend product, comprise one with the pipe shaft of feeding mouth and separating opening, the separating opening of this fiber separation device downwards and with cock, is 30 ~ 80 ° along the tilt angle alpha of sideline and perpendicular line under the inside pipe wall of pipe shaft.
Pipe shaft length in described fiber separation device is (50 ~ 100) with the ratio of the mouth internal diameter size of separating opening: 1.Preferably (60 ~ 80): 1, pipe shaft length is 200 ~ 400mm, and tube body diameter is 40 ~ 50mm; The mouth internal diameter size of described separating opening is 3 ~ 5mm.
The present invention mainly for the quantitative test of the fiber content of natural bamboo fibres and other cellulosic fibre blend products, and proposes a kind of device for the method.The inventive method can be extended in the fiber content quantitative test of flaxen fiber or cotton fiber and other cellulosic fibre blend products simultaneously.
Density gradient separation liquid in the present invention is the special dispense liquid of a series of density gradual change, carry out larger improvement for existing fiber separation device simultaneously, redesign the angle of inclination of the end inwall of fiber separation device and the important parameter such as caliber size, pipe shaft length of separating opening.Wherein, pipe shaft effect length the validity of sample separation, effective pipe shaft length, widened the two ends density distance of density gradient separation liquid, thus each fiber in the sample making density variation less still effectively can be separated; Can the tube body diameter angle of inclination at separating opening place and separating opening caliber size affect precipitation fiber leave separating opening smoothly.Otherwise the sample measured cannot be separated, be separated after fiber cannot discharge separating opening smoothly, finally affect the accuracy of test result.The density gradient separation liquid that the present invention proposes for this reason matches with the fiber separation device that the present invention proposes, and just density closely two kinds of fibers effectively can be separated.
Advantage of the present invention is:
1. present invention achieves performance interfibrous separation closely, be specially adapted to natural fiber as the separation between native cellulose fibre, and comparatively prior art, can more high-precision mensuration be carried out;
2. what the present invention adopted is that the fiber in sample is separated by a kind of physical method and a kind of fiber separation device separately with no damage, therefore without the need to revising any one result;
3. simple, convenient; Realize method of the present invention and installation cost low;
4. the method applicable object is wide, and the accuracy rate of quantitative test is high.
Accompanying drawing explanation
Fig. 1 is the structural representation (analysing and observe) of fiber separation device of the present invention.
Embodiment
The concrete steps of the preferred implementation method of fiber content assay method one of the cellulosic fibre blend product that the present invention is one of raw material with bamboo fibre, flaxen fiber or cotton fiber are as follows:
1. the pre-service of material:
1) finished product of fabric, semi-manufacture are through spinning, spinning, textile process process inevitably more residual non-fibrous materials, and grease, wax or finishing agent etc. mainly on fiber or fabric, the existence of these materials will have a strong impact on density measurement.For avoiding error, need before test to remove these non-fibrous materials, petroleum ether extraction method (with reference to Beijing: China Standards Press .2009 publishes the appendix A in " quantitative test of GB/T2910.1-2009 textile chemistry " standard) can be adopted to carry out removing the pre-service of non-fibrous material to the finished product of fabric, semi-manufacture, and concrete grammar is as follows:
Getting appropriate amount of sample is placed in soxhlet's extractor, with sherwood oil (analyzing pure) extraction 1h, and at least circulation per hour 6 times, the ratio of bath raio 1: 100(sample and sherwood oil liquid), temperature 40-60 DEG C.
After the sherwood oil volatilization in sample, sample is immersed in 30min-1h in cold water, then soaks 1-2h, agitating solution in immersion process in the water of (65 ± 5) DEG C, extract, suction filtration or centrifugal dehydration, natural drying, stand-by.
2) for bast class native cellulose fibre, if need to remove colloid, preprocess method is as follows:
Sample is immersed in by the mixed liquor of hydrogen peroxide (mass percent concentration concentration is 30%) and glacial acetic acid (mass percent concentration is not less than 99.5%) 1: 1-1: 4 proportions by volume, under the treatment temperature of 60-80 DEG C, be vibrate in 80-100r/min water-bath constant temperature oscillator at rotating speed, processing time is 24-30h, extract, suction filtration or centrifugal dehydration, natural drying, stand-by.
2. the preparation of material and requirement:
Get pretreated sample (0.5 ± 0.1g)/part and cut into 1 element length (being 0.5-1mm in the present embodiment), dry, fully get rid of bubble, cooling is weighed, the total dry mass after the oven dry of record sample, the sample after weighing is deposited in dry vessel.
3. the preparation of density gradient separation liquid:
At field of textiles, densimetry can be used for the Qualitive test of fiber, and the liquid of a certain density can be used for the separation of two kinds of larger fibers of performance difference; Density gradient can be used for the mensuration of fibre density.When test the mutual performance of fiber in sample closely time, the separation thickness of each fiber, the separating layer of two kinds of fibers are obscured mutually, it is unclear to be separated, and therefore the liquid of a certain density cannot be used for the fiber separation in the blending products such as fibre density cotton closely, fiber crops, viscose and bamboo fibre.Because the cellulose fibre properity difference that particularly native cellulose fibre is mutual is very little, and with regard to a kind of natural fiber, the mutual density of fiber also has certain discrete.The liquid-tight degree of density gradient separation of the present invention is the special liquid of a series of continuous print density gradual change of (from bottom to top) from big to small, and in this liquid, two kinds of density fiber closely distance that rises and falls up and down is strengthened, thus ensures to be separated exactly.Can be used for reagent prepared by density gradient separation liquid of the present invention to have: phenixin (1.595g/cm
3), methenyl choloride (1.484/cm
3), methylene chloride (1.336g/cm
3); Dimethylbenzene (0.865g/cm
3), toluene (0.871g/cm
3), normal heptane (0.695g/cm
3) etc., be analysis pure.
When the sample of the present invention to the cellulosic fibre blend product being one of raw material with bamboo fibre, flaxen fiber or cotton fiber carries out fiber content mensuration, two kinds of liquid configurations of mentioned reagent can be selected as required.Such as: the density knowing contained two kinds of cellulose fibres in surveyed blending product in advance, select the mentioned reagent of two kinds of density to carry out configuration density gradient separations liquid, the density of this density gradient separation liquid will in this sample two kinds of fibers density between.
As known in advance in this blending product containing first, second, and third totally three kinds of cellulose fibres, then prepared two groups of density gradient separation liquid by the density of the three kinds of cellulose fibres calibrated according in this sample, wherein the density of one group of density gradient separation liquid is between the density of the first and second two kinds of cellulose fibres; The density of another group density gradient separation liquid is between second and the density of the 3 two kind of cellulose fibre, and the density of two groups of density gradient separation liquid becomes large from top to bottom gradually, and continuous distribution forms gradient.
4. the preparation of instrument, articles for use:
Experimental apparatus and articles for use: constant temperature water bath (with heating constant-temperature equipment and stirring apparatus, height is suitable with fiber separation device height), water circulating pump, fiber separation device (special), magnetic stirring apparatus, flat Erlenmeyer flask and two siphunculus, filtration unit, nutsch filter, densitometer, graduated cylinder, test tube;
Experiment condition: 20 ± 0.5 DEG C
Fiber separation device concrete structure of the present invention can see Fig. 1, and its main composition is one with the pipe shaft 1 of feeding mouth 2 and separating opening 3, and the separating opening of this fiber separation device downwards and with cock 4, cock is reversed and opened or closed separating opening.It seems similar to common tripping device, but the mouth internal diameter size (3-5mm) of the bore tilt angle alpha (30-80 °) of fiber separation device pipe shaft 1 lower end, separating opening 3, pipe shaft 1 length (200-400mm), pipe shaft 1 internal diameter (40-50mm), pipe shaft length are all important parameters with the ratio (50-100: 1) etc. of the caliber size of separating opening.Wherein pipe shaft effect length the validity of fiber separation in sample, effective pipe shaft length, has widened the two ends density distance of density gradient separation liquid, thus the very little fiber of sample Midst density difference still can be effectively separated; Can the tube body diameter angle of inclination at separating opening place and separating opening caliber size affect precipitation fiber leave separating opening smoothly.Otherwise the sample measured cannot be separated, be separated after fiber cannot discharge separating opening smoothly, finally affect the accuracy of test result.During use, a becket 5 can be placed in the inwall lower end of fiber separation device feeding mouth 2, with ensure drip reagent can along wall and under.
5. the separation of two or more composite fibre in sample:
Testing sample to be inserted in the fiber separation device having configured density gradient separation liquid (constant temperature water bath that tripping device is placed in 20 ± 0.5 DEG C keep temperature constant constant), this fiber separation device is with openable separating opening, one filtration unit of weighing is in advance set in the below of fiber separation device separating opening, overall standing 30-60min, the fiber that in sample, contained density is less is floated, and the fiber sinking that density is larger.After both are separated, the separating opening of knob Unscrew fiber separation device, the fiber sunk after leaving standstill can be separated in the filtration unit of known weight with density gradient separation liquid.
Equally, method roughly the same can be taked, kind of the composite fibre of 3 in sample be isolated a kind or 2 kinds of fibers, finally can obtain the dry weight of 2 kinds of fibers.
6. the fiber content completing sample measures and calculates:
According to formula-1, formula-2, formula-3 calculate respectively the first, the third and the second fiber content:
(formula-2)
The second fiber content (%)=the third fiber content of the first fiber content of 100%-(%+ %).
(formula-3)
Be no matter the blending product of 2 kinds or 3 kinds fibers, all record fiber content by the inventive method.
Principle of the present invention is:
(1) when the chemical composition of cellulose fibre is identical or close time, physical arrangement (particularly supramolecular structure) affects the key factor that fibre property comprises density.The crystallinity of fiber is higher, and supramolecular structure is tightr, and the density of fiber is larger; Vice versa.Result of study shows: no matter native cellulose fibre or regenerated celulose fibre, all different in its supramolecular structure, thus causes the density of various cellulose fibre all not identical.
(2) density gradient separation of the present invention utilizes the density variation between two kinds of (or more than three kinds) fibers, the potpourri of two kinds of (or more than three kinds) fibers is placed in the liquid of certain a series of density, obtain upper lower leaf by floating and precipitate, thus be separated.Require for separating of the density of this density gradient separation liquid between two kinds of fibers (during more than three kinds fibers, two adjacent fibers by after the arrangement of density size order) between density, and density from top to bottom becomes large gradually, and continuous distribution forms gradient; In addition, this density gradient separation liquid does not all affect measured fiber and damages.
(3) except supramolecular structure is on except the impact of fibre density, for bast fibers, the existence of colloid also has a significant impact fibre density test result, because colloid is amorphous state, therefore the density measurement value containing the bast fiber of colloid is declined.Such as: bamboo fibre, also comprise all containing a large amount of colloids in the bast such as flax, jute class raw ramie fiber, gum level is relevant with the degumming degree of fiber.If two kinds of interfibrous density variations therefore will be strengthened, to make two kinds of fibers be separated because Relatively density contrast is comparatively large, the fiber coming unstuck or do not come unstuck can be adopted intentionally, as the bamboo fibre that do not come unstuck and cotton fiber density variation between the two larger than the density variation between the bamboo fibre come unstuck and cotton fiber.
Below in conjunction with specific embodiment, the present invention is described further.
Embodiment one: the fiber content quantitative test in bamboo fibre and cotton fiber blending product.
Concrete steps are as follows:
First sample is prepared by the method for above-mentioned pretreatment; Density gradient separation liquid is prepared: first use phenixin (1.595g/cm in density range again between bamboo fibre and cotton fiber
3), normal heptane (0.695g/cm
3) two kinds of reagent configure 150ml light liquid respectively (density is: 1.525g/cm
3; With 138.3ml phenixin+11.7ml normal heptane configuration) and 150ml heavy-fluid (density is: 1.535g/cm
3; With the configuration of 140.0ml phenixin+10.0ml normal heptane), the steel wire ring that one matches with the internal diameter of fiber separation device feeding mouth is placed in the inwall lower end of feeding mouth, the heavy-fluid prepared above-mentioned, light liquid inject fiber separation device successively continuously, rate of addition 8 ~ 10mL/min, fiber separation device internal wall of pipe orifice is close to when dripping liquid, make heavy-fluid, light liquid inject fiber separation device along steel wire ring successively, make density at 1.525 ~ 1.535g/cm
3density gradient separation liquid (closely about 300ml).
The above-mentioned tripping device filling density gradient separation liquid is placed in the constant temperature water bath of 20 ± 0.5 DEG C, and keeps temperature constant constant, to sample without the need to degumming process.
Sample is inserted and above-mentionedly fills in the tripping device of density gradient separation liquid, overallly leave standstill 40min, the bamboo fibre that in sample, contained density is less is floated, and the larger cotton fiber of density sinks.Both are separated completely, open the separating opening of fiber separation device, and the cotton fiber sunk after leaving standstill can be separated in filtration unit with density gradient separation liquid, and dry process, records isolated cotton fiber dry weight; Again by the bamboo fibre separation remained in fiber separation device, dry process, record bamboo fibre dry weight, obtains one group of experimental data.Adopt the parallel laboratory test being no less than 3 groups, the blending ratio of bamboo fibre/cotton fiber mixed yarn is tested, to reduce experimental error.Get 5 groups of experimental results to list in table 1.
Table 1 density gradient separation is to the measurement result of bamboo fibre/cotton fiber mixed yarn blending ratio
The former blending ratio design proportion of this test sample bamboo fibre/cotton fiber mixed yarn is 40:60, is 40.1:59.9 through method test result of the present invention, proves that the test accuracy rate of the bamboo fibre/cotton fiber mixed yarn blending ratio obtained is very high.
The bamboo fibre of embodiment two: two kinds of different designs ratios and the fiber content quantitative test of tossa blending product
Adopt the assay method being analogous to embodiment one, with phenixin (1.595g/cm
3) and dimethylbenzene (0.865g/cm
3) two kinds of reagent first configure 130ml light liquid (109.5ml phenixin+20.5ml dimethylbenzene), 130ml heavy-fluid (113.1ml phenixin+16.9ml dimethylbenzene), then by light liquid, heavy-fluid preparation density at 1.480 ~ 1.500g/cm
3density gradient separation liquid (about 250ml) in scope, adopts the parallel laboratory test being no less than 3 groups, tests in the blending ratio of method of the present invention to the bamboo fibre/tossa mixed yarn (sample is without the need to degumming process) of two kinds of different designs ratios.In density gradient separation liquid, bamboo fibre sinks, tossa floats.The test result of two groups lists in table 2 altogether.
Table 2 density gradient separation is to the measurement result of the bamboo fibre/jhouta blended yarn blending ratio of different proportion
As seen from the results in Table 2, design blending ratio is the test result of the bamboo fibre/tossa mixed yarn of 40:60 is 39.2:60.8, and accuracy rate is very high; And the fiber content test result designing the bamboo fibre/tossa mixed yarn of blending ratio 70:30 is 67.8:32.2, result error is slightly large.But it is noted that the blending product due to bamboo fibre is still unstable on spinning process here, between the actual blending ratio of bamboo fiber blended product and design blending ratio, still have certain error.
Embodiment three: the fiber content quantitative test of ramee and viscose fiber blending product
Table 3 density gradient separation is to the measurement result of ramie/viscose mixed yarn blending ratio
Adopt the assay method being analogous to embodiment one, in special fiber separation device, prepare one group of density at 1.515 ~ 1.540g/cm
3density gradient separation liquid in scope, be that the sample after the process of 30:70 ramee/viscose fiber mixed yarn drops into wherein by design blending ratio, this group density gradient separation liquid can by phenixin (1.595g/cm
3) and methenyl choloride (1.484/cm
3), methylene chloride (1.336/cm
3), dimethylbenzene (0.865g/cm
3), toluene (0.871g/cm
3) and normal heptane (0.695g/cm
3) in a kind of reagent mixed preparing.
Measure by method of the present invention, the measurement result of this mixed yarn blending ratio is listed in table 3, result is ramie: viscose 30.2:69.8, and illustrate that density gradient separation can be separated with the blending product of viscose fiber very accurately to ramee, variance is 0.43596%.
Embodiment four: the fiber content quantitative test of ramee and flax fiber blending product
Prepare one group of density at 1.538 ~ 1.545g/cm
3density gradient separation liquid in scope, sample is without the need to degumming process, and the fiber content quantitative analysis results of the ramie/flax blended spinning of different proportion is as shown in table 4.
Table 4 density gradient separation is to the test result of ramie/flax blended spinning blending ratio
Table 4 is the results adopting the ramie/flax blended spinning of density gradient separation to two kinds of different proportions to carry out quantitative test.Can find out: density gradient separation is accurately for the quantitative test of fiber content in mixed yarn, differ within 1% with design blending ratio, variance <1%.
Embodiment five: the fiber content quantitative test of cotton fiber and Lyocell fiber blending product
Table 5 density gradient separation is to the measurement result of 70/30 cotton/Lyocell fiber mixed yarn blending ratio
Preparation density is at 1.530 ~ 1.535g/cm
3density gradient separation liquid in scope, the quantitative analysis results of cotton after pretreatment/Lyocell fiber blending product sample is listed in table 5, and result shows test blending ratio and design the difference of blending ratio within 0.05%.
Embodiment six: the fiber content quantitative test of bamboo fibre/cotton fiber/viscose fiber blending product
By aforementioned the present invention prepared by material degumming pretreatment method to the sample of this blending product.Then, phenixin (1.595g/cm is adopted
3), toluene (0.871g/cm
3) first two kinds of reagent prepare density at 1.525 ~ 1.535g/cm
3density gradient separation liquid in scope, separates the cotton fiber in pretreated blended sample, dry process, record dry weight; Use phenixin (1.595g/cm and then
3), toluene (0.871g/cm
3) two kinds of preparation of reagents density are at 1.515 ~ 1.520g/cm
3density gradient separation liquid in scope, or also can at methenyl choloride (1.484/cm
3), methylene chloride (1.336g/cm
3), dimethylbenzene (0.865g/cm
3), toluene (0.871g/cm
3) and normal heptane (0.695g/cm
3) in select a kind of reagent and phenixin (1.595g/cm
3) reagent mixed preparing density is at 1.515 ~ 1.520g/cm
3density gradient separation liquid in scope; Bamboo fibre in blended sample after the pre-service of resampling and cotton fiber are separated, viscose fiber remains in fiber separation device, is isolated by residue viscose fiber and dry process, record dry weight.Density gradient separation measures the fiber content of bamboo fibre/cotton fiber/viscose fiber blending product and result of calculation is listed in table 6.
Table 6 density gradient separation is to the measurement result of bamboo fibre/cotton fiber/viscose fiber mixed yarn blending ratio
The various embodiments described above can in addition some changes under not departing from the scope of the present invention, therefore above explanation comprises and should be considered as exemplary, and is not used to the protection domain limiting the present patent application patent.
Claims (9)
1. a fiber content assay method for cellulosic fibre blend product, has known containing two kinds of cellulose fibres in this blending product, and at least containing the one in bamboo fibre, flaxen fiber and cotton fiber; It is characterized in that method step is as follows:
A) pre-service of removing non-cellulosic material is carried out to the sample of cellulosic fibre blend product to be measured;
B) get a pretreated 1 element length sample, after final drying, record its total dry mass, stand-by;
C) in fiber separation device, density gradient separation liquid is prepared by the density of the two kinds of cellulose fibres calibrated according in this sample, between the density of density two kinds of cellulose fibres in this sample of this density gradient separation liquid, and the density of parting liquid becomes large from top to bottom gradually, and continuous distribution forms gradient; With openable separating opening bottom this fiber separation device, a filtration unit of weighing is in advance set in the below of fiber separation device separating opening; Described fiber separation device comprises one with the pipe shaft of feeding mouth and separating opening, and the separating opening of this fiber separation device is with cock; When described pipe shaft uses, its separating opening is downward, and is 30 ~ 80 ° along the tilt angle alpha of sideline and perpendicular line under the inside pipe wall at the nearly separating opening place of pipe shaft; Pipe shaft length is 200 ~ 400mm, and tube body diameter is 40 ~ 50mm, and the mouth internal diameter size of separating opening is 3 ~ 5mm, and pipe shaft length is (60 ~ 80) with the ratio of the mouth internal diameter size of separating opening: 1;
D) after the preparation of density gradient separation liquid terminates, testing sample is inserted in fiber separation device; Overall standing 30-60min;
E) open the separating opening bottom fiber separation device, the first fiber sunk after leaving standstill is separated in filtration unit with density gradient separation liquid;
F) by the first fiber drying process isolated, the first fiber dry weight isolated is recorded;
G) by the second fiber separation remained in fiber separation device, dry process, record the second fiber dry weight;
H) the various fiber contents of this cellulosic fibre blend product are calculated:
2. the fiber content assay method of cellulosic fibre blend product according to claim 1, it is characterized in that: the concrete preparation of described density gradient separation liquid: light, the heavy-fluid preprepared with two kinds of different densities inject fiber separation device according to the secondary Order continuous that density is descending, rate of addition 8 ~ 10mL/min, wherein, light liquid density is greater than the density of the light fiber in sample, and heavy-fluid density is less than the density of the heavy fiber in sample.
3. the fiber content assay method of cellulosic fibre blend product according to claim 2, is characterized in that: the light or heavy-fluid of described preparation density gradient separation liquid is by two kinds of liquid mixed preparing in phenixin, methenyl choloride, methylene chloride, dimethylbenzene, first benzene and heptane; During preparation density gradient separation liquid, the feeding mouth inwall need being close to fiber separation device drips liquid, place a steel wire ring identical with spout diameter size in the feeding mouth inwall lower end with tapering of fiber separation device, make heavy-fluid, light liquid inject fiber separation device along steel wire ring successively.
4. the fiber content assay method of cellulosic fibre blend product according to claim 1, it is characterized in that: described fiber separation device is prepended in the constant temperature water bath of 20 ± 0.5 DEG C in the preparation of density gradient separation liquid, and continue in mensuration, to keep temperature constant constant, until the fiber fractionation in sample.
5. the fiber content assay method of a cellulosic fibre blend product, know containing first, second, and third totally three kinds of cellulose fibres by the descending sequence of density in this blending product, and at least containing the one in bamboo fibre, flaxen fiber and cotton fiber; It is characterized in that method step is as follows:
A) pre-service of removing non-cellulosic material is carried out to the sample of cellulosic fibre blend product to be measured;
B) get the sample of two parts of pretreated 1 element lengths, after final drying, record total dry mass of every increment product, stand-by;
C) according in this sample by the density of three kinds of cellulose fibres calibrated, preparation first and second liang group density gradient separation liquid in the first and second two fiber separation devices respectively, the density of each group of density gradient separation liquid becomes large from top to bottom gradually, and continuous distribution forms gradient; Wherein: the density of first group of density gradient separation liquid is between the density of the first and second two kinds of cellulose fibres, and the density of second group of density gradient separation liquid is between second and the density of the 3 two kind of cellulose fibre; Described fiber separation device comprises one with the pipe shaft of feeding mouth and separating opening, and the separating opening of this fiber separation device is with cock; When described pipe shaft uses, its separating opening is downward, and is 30 ~ 80 ° along the angle of inclination of sideline and perpendicular line under the inside pipe wall at the nearly separating opening place of pipe shaft; Pipe shaft length is 200 ~ 400mm, and tube body diameter is 40 ~ 50mm, and the mouth internal diameter size of separating opening is 3 ~ 5mm, and pipe shaft length is (60 ~ 80) with the ratio of the mouth internal diameter size of separating opening: 1;
D) two parts of testing samples are inserted respectively in the first and second two fiber separation devices, add rear respective entirety and leave standstill 30-60min;
E) separating opening bottom two fiber separation devices is opened respectively, wherein: the first fiber sunk after leaving standstill in the first fiber separation device is separated in the filtration unit of weighing be in advance preset at below the first fiber separation device separating opening with first group of density gradient separation liquid; The first of sinking after leaving standstill in the second fiber separation device is separated to second group of density gradient separation liquid in the filtration unit of weighing be in advance preset at below the second fiber separation device separating opening jointly with the second fiber, and the third fiber has remained in the second fiber separation device;
F) its dry weight is recorded in the first fiber drying process isolated in the first fiber separation device; The third fiber separation remained in the second fiber separation device, drying are processed and record its dry weight;
G) three kinds of fiber contents of this cellulosic fibre blend product are calculated:
The second fiber content (%)=100%-(the third fiber content of the first fiber content %+ %).
6. the fiber content assay method of cellulosic fibre blend product according to claim 5, it is characterized in that: the concrete preparation of described first group of density gradient separation liquid: light, the heavy-fluid preprepared with two kinds of different densities inject the first fiber separation device according to the secondary Order continuous that density is descending, rate of addition 8 ~ 10mL/min, wherein, light liquid density is greater than the density of the second cellulose fibre in sample, and heavy-fluid density is less than the density of the first cellulose fibre in sample; The concrete preparation of second group of density gradient separation liquid: light, the heavy-fluid preprepared with two kinds of different densities inject the second fiber separation device according to the secondary Order continuous that density is descending, rate of addition 8 ~ 10mL/min, wherein, light liquid density is greater than the density of the third cellulose fibre in sample, and heavy-fluid density is less than the density of the second cellulose fibre in sample.
7. the fiber content assay method of cellulosic fibre blend product according to claim 6, is characterized in that: the light or heavy-fluid of described preparation density gradient separation liquid is by two kinds of liquid mixed preparing in phenixin, methenyl choloride, methylene chloride, dimethylbenzene, first benzene and heptane; During preparation density gradient separation liquid, the feeding mouth inwall need being close to fiber separation device drips liquid, place a steel wire ring identical with spout diameter size in the feeding mouth inwall lower end with tapering of fiber separation device, make heavy-fluid, light liquid inject fiber separation device along steel wire ring successively.
8. the fiber content assay method of cellulosic fibre blend product according to claim 5, it is characterized in that: when described sample is the blending product of the native cellulose fibre of bast class, the process of colloid need be removed to sample: sample is immersed in mass percent concentration be 30% hydrogen peroxide and mass percent concentration glacial acetic acid 1: 1 ~ 1: 4 proportions by volume that are not less than 99.5% mixed liquor in, under the treatment temperature of 60 ~ 80 DEG C, be vibrate in 80 ~ 100r/min water-bath constant temperature oscillator at rotating speed, processing time is 24 ~ 30h, extract, suction filtration or centrifugal dehydration, natural drying, stand-by.
9. the fiber content assay method of cellulosic fibre blend product according to claim 5, it is characterized in that: described fiber separation device is prepended in the constant temperature water bath of 20 ± 0.5 DEG C in the preparation of density gradient separation liquid, and continue in mensuration, to keep temperature constant constant, until the fiber fractionation in sample.
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| CN107063917A (en) * | 2017-06-29 | 2017-08-18 | 莱茵技术-商检（青岛）有限公司 | A kind of method for determining cellulose fiber content in the natural or two-component mixture of regenerated celulose fibre and polyester fiber |
| CN107356493A (en) * | 2017-07-12 | 2017-11-17 | 北京和众视野科技有限公司 | Textile fiber content automatic calculating method |
| CN111912733A (en) * | 2020-08-12 | 2020-11-10 | 威海拓展纤维有限公司 | Method for testing mass fraction of fibers in carbon fiber reinforced nylon plastic |
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