CN104764736B - Lyocell A100 discrimination method and its application - Google Patents
Lyocell A100 discrimination method and its application Download PDFInfo
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- CN104764736B CN104764736B CN201510143405.5A CN201510143405A CN104764736B CN 104764736 B CN104764736 B CN 104764736B CN 201510143405 A CN201510143405 A CN 201510143405A CN 104764736 B CN104764736 B CN 104764736B
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Abstract
The present invention relates to a kind of method for differentiating lyocell A100 from regenerated celulose fibre, the sample of the A100 containing lyocell is dissolved using formic acid/liquor zinci chloridi, and whether the insoluble matter of observation dissolving reaction, qualitative detection contains lyocell A100；Present invention application of the discrimination method in lyocell A100 detections simultaneously.The discrimination method of the present invention fast and accurately can identify lyocell A100 from other regenerated celulose fibres, be a kind of strong qualitative identification method of exploitativeness, while established the basis of lyocell A100 quantitative analyses.
Description
Technical field
The invention belongs to fibre identification technical field, and in particular to differentiate lyocell A100's from regenerated celulose fibre
Method, while it is related to its application in lyocell A100 discriminatings.
Background technology
Due to the reduction in arable land and the increasingly depleted of petroleum resources, natural fiber, the yield of synthetic fibers are by increasingly
More restrictions, for people while textile environmental-protecting performance is paid attention to, the development and utilization to regenerated celulose fibre is increasingly heavier
Depending on.Regenerated celulose fibre belongs to native cellulose regenerated fiber, and its structure composition and cotton fiber are quite similar, but have cotton
Excellent performance as the silk that fiber does not possess, regenerated celulose fibre are a kind of function admirable " green " fibers, its
Waste and old gurry can natural degradation.Regenerated celulose fibre is the direction of future development, is the effective way for solving natural resources shortage
Footpath.
Regenerated celulose fibre refers to by cotton linter, straw, beech, eucalyptus, bamboo etc. be renewable, degradable, ring
The native cellulose class raw material of guarantor, by special process production can be used in weaving tencel, these fibers it is basic
Composition is cellulose II.Mainly have：The common viscose fiber to emerge early 20th century, the koplon of the fifties, copper
Ammonia fiber；The Modal fibre in the Lenzin company later stage eighties；The more excellent Lyocell fibers of commercialization nineties performance；Last century
Bamboo pulp fiber of last China's invention etc..Their general character：Manufacture raw material（Base material）Property is close --- native cellulose；Technique phase
Closely --- cellulose dissolution spinning again；Molecular structure is similar --- macromolecular cellulose II；Chemical property-the dissolving of fiber in itself
Performance is similar.Their difference：Only molecular weight is slightly different, slightly different for physical property, but wearing comfort has very very much not
Together, price has notable difference.Due to so many similar so that carrying out accurate qualitative and quantitative analyses to them turns into current
One of generally acknowledged problem in textile fiber composition detection field in world wide.
Fiber content detection be domestic and international technical regulation compulsory test project, in recent years, textile fabric mark composition with
The consumption fraud problems that reality is not consistent are very universal, account for textile product nonconformance purpose more than 80%.Particularly, in recent years
The appearance of tencel, because these fibrous raw material price variances are larger, these fraud problems of prevention and control are new there is an urgent need to develop
Detection technique, what the discriminating coherent detection field to this fiber was being done one's utmost always studies, but at home and abroad all
There is not yet correlative regeneration fiber blending products composition detection, the report of effective and feasible detection method.With scientific and technological progress, then
The species of raw cellulose fibre is also being continuously increased, and it differentiates, detection technique is badly in need of haveing breakthrough.Than regeneration as mentioned above
The discriminating of cellulose fibre just detects foundation with quantitative analysis without effective method and reliably, so as to mix the spurious with the genuine,
The problem of dolus malus consumer, is very universal, and therefore, invention is a kind of to differentiate Lyocell fibers from regenerated celulose fibre
Method is very urgent, there is extremely important realistic meaning.What regenerated celulose fibre had largely used at present has：It is common viscous
Glue fiber, Modal, lyocell, bamboo fibre etc..
Lyocell fibers are divided into lyocell A100, lyocell LF, tri- kinds of lyocell G100 according to its production technology difference,
But in actual application, cotton mill all specializes the species of lyocell when purchasing raw material, and is only marked after being manufactured into clothes
Bright is Lyocell fibers.Because the property of three kinds of lyocells is similar, it is not enough to effectively distinguish with current classical discrimination method, again
Because the chemical property of three kinds of lyocells is seemingly different, cause a problem occurs in detection process：The Lay equally indicated
The product of Sai Er fibers and some fiber blends, when doing fiber content detection, detection data are unstable, and main cause is exactly not
Lyocell A100, lyocell LF, lyocell G100 difference of the same clan can accurately be differentiated, do not know where to begin more lyocell A100 and other
The quantitative analysis method of regenerated celulose fibre.
The content of the invention
It is simple, high sensitivity from regenerated celulose fibre that the technical problems to be solved by the invention are to provide a kind of flow
It is middle to differentiate lyocell A100 method, while its application is provided.
The present invention solve the technical scheme that uses of its technical problem for：A kind of lyocell A100 discrimination method, from regeneration
Differentiate lyocell A100 in cellulose fibre, comprise the following steps：
（a）Prepare formic acid/liquor zinci chloridi：Take 18-25 grams of zinc chloride with（70±2）Gram formic acid, add water quantitative to 100
Gram；
（b）The regenerated celulose fibre sample of the fibers of A100 containing lyocell is added into step（a）In resulting solution, in 67-
18-25 minutes are vibrated at 80 DEG C；
（c）Observation of steps（b）Dissolving result, insoluble matter is lyocell A100.
Preferably, sample and formic acid/liquor zinci chloridi mass ratio are 1:100.
Preferably, step（b）The frequency of the vibration is 100 beats/min.
Preferably, the zinc chloride is powdered.
Preferably, step（c）Solution is poured into the stainless steel mesh of 100 mesh during observation.
Preferably, step（b）Sample rear 67-72 DEG C of temperature holding after adding, vibrates 18-25 minutes.
Present invention simultaneously provides application of the discrimination method in lyocell A100 is differentiated.
The positive effect of the present invention is that the invention provides a kind of lyocell A100 Qualitive test side
Method, lyocell A100 can be identified from other regenerated celulose fibres using the method for the present invention, required preparation of reagents
Simply, in the reaction time provided by the invention with a temperature of, discrimination threshold is high, and exploitativeness is strong.
The invention provides formic acid/liquor zinci chloridi to differentiate application of the method for fiber in lyocell A100 is differentiated, GB/
Formic acid/zinc chloride differentiates cotton and Lyocell fibers in T2910.6-2009, and therefore, Lyocell fibers are dissolved in standard
Formic acid/liquor zinci chloridi is the common knowledge of those skilled in the art.It is unexpected but the present inventor is in concrete operations
It was found that lyocell A100 does not dissolve in formic acid/liquor zinci chloridi, lyocell A100 dissolubility and regenerated fiber under certain condition
Cellulose fiber has nuance in the dissolution conditions of formic acid/liquor zinci chloridi, investigates, finally determines by many experiments and repeatedly
It differentiates lyocell A100 optimum condition, provides application of the discrimination method in lyocell A100 discriminatings in a creative way.
Embodiment
In order to facilitate the understanding of the purposes, features and advantages of the present invention, below in the embodiment of the present invention
Technical scheme be clearly and completely described, it is clear that described embodiment is only part of the embodiment of the present invention, and
The embodiment being not all of.Based on the embodiment in the present invention, those of ordinary skill in the art are not making creative work
Under the premise of the every other embodiment that is obtained, belong to the scope of protection of the invention.
In technical solution of the present invention, formic acid/liquor zinci chloridi, gained are prepared with 68 grams of anhydrous formic acids and 80 gram of 88% formic acid
Every testing result is respectively provided with uniformity.
Embodiment 1 differentiates lyocell A100 from regenerated celulose fibre
The specific method of embodiment 1 is：18-25 grams of anhydrous zinc chloride powder and 68 grams of anhydrous formic acids are taken, adds water quantitative to 100
Gram, prepare formic acid/liquor zinci chloridi.Formic acid/liquor zinci chloridi is first added in tool fills in conical flask, places into measuring samples,
The sample is 1 with formic acid/liquor zinci chloridi mass ratio:100, bottle stopper is covered, vibrates 20min at 70 DEG C, pours into 100 purposes
In stainless steel mesh, residue has been checked whether.Remaining insoluble matter is lyocell A100.
The measuring samples of embodiment 1 are 6 groups, and sample is obtained by mixing using known fiber, and the concrete composition of sample is shown in Table 1；
After discrimination method reacts, the quality and identification result of the anhydrous zinc chloride that 6 groups of samples are selected when dissolving are shown in Table 1.It can be seen that this reality
The testing result of the discrimination method of example is applied with actual consistent, accuracy rate is higher.
The composition of each sample of 1 embodiment of table 1, detection use the amount and testing result of zinc chloride
Note：" √ " represents to contain the composition.
The reagent of experimental example 1 selects
The primary solvent for typically differentiating cellulose fibre with dissolution method has sulfuric acid, hydrochloric acid, nitric acid, copper ammon solution, quantitative
Sulfuric acid, formic acid liquor zinci chloridi are commonly used in analysis, also uses zincic acid sodium solution, sodium hydroxide/thiocarbamide/urea liquid etc. sometimes.
By the use of formic acid liquor zinci chloridi as Qualitive test reagent still first.
Reagent in experimental example 1 is prepared according to the proportioning of table 2, in the bath raio shown in table 2, temperature, time, oscillation frequency
Tested under rate, as a result such as table 2.
Dissolubility of the 2 various regenerated celulose fibres of table in reagent
Conclusion：
1) formic acid/zinc chloride be by lyocell A100 and other regenerated celulose fibres it is fast, sensitive be distinguished
Optimal reagent.
2) sodium hydroxide/thiocarbamide/urea reagent cannot differentiate lyocell A100 and lyocell LF, lyocell G100
Come.
3) four kinds of sulfuric acid, hydrochloric acid, nitric acid, copper ammon solution solution are the discriminating celluloses that FZ/T 01057.3-2007 are listed
The reagent of fiber, but they can not by lyocell A100 with other regenerated celulose fibres are qualitative is distinguished.
Therefore, lyocell A100 and other regenerated fibers when testing primary study using formic acid/zinc chloride as solvent below
The optimal conditions selection that cellulose fiber differentiates.
The selection of 2 formic acid of experimental example/chlorination zincon ratio range and optimal proportion
At 70 DEG C, according to the reagent preparation of table 3, reaction time 20min, the solubility property of each regenerated celulose fibre are dissolved
It is shown in Table 3.
The solubility property of each regenerated celulose fibre under 3 different reagents of table proportioning
Conclusion：
1) certain density formic acid/zinc chloride can be all molten by regenerated celulose fibres such as viscose glue, Modal, bamboo fibres
Solution.
2）When zinc oxide concentration is too low in formic acid, it is impossible to distinguish three kinds of Lyocell fibers, only when zinc chloride reaches
During certain concentration, lyocell LF and lyocell G100 can be just completely dissolved, remaining lyocell A100.
3）Differentiate that chlorination Zn content at least should be 20g/100g in formic acid/zinc chloride that lyocell A100 is used, it is contemplated that
Environmental protection and the principle of easy operation, the compound method of formic acid/zinc chloride is 20g anhydrous zinc chlorides（Mass fraction ＞ 98%）Add
Into 80g 88% formic acid.
The temperature-time scope of experimental example 3 selects
20 grams of anhydrous zinc chloride powder and 68 grams of anhydrous formic acids are taken, adds water quantitative to 100 grams, it is molten to prepare formic acid/zinc chloride
Liquid.Formic acid/liquor zinci chloridi is first added in tool fills in conical flask, places into measuring samples, the sample and formic acid/zinc chloride
Solution quality ratio is 1:100, bottle stopper is covered, is vibrated under temperature and time shown in table 4, is poured into the stainless steel mesh of 100 mesh,
Residue has been checked whether, the results are shown in Table 4.
The solubility property of each regenerated celulose fibre under the different temperature and time of table 4
Conclusion：
1）When temperature is relatively low, Lyocell fibers are all relatively stable, not readily dissolve, thus can by viscose glue, Modal and
Bamboo fibre is distinguish between with Lyocell fibers.
2）With the rise of temperature, the rate of dissolution of viscose glue, Modal and bamboo fibre is accelerated, within a short period of time can be with molten
Solution is complete, but lyocell A100, lyocell G100 and lyocell LF are difficult to differentiate between.
3）When temperature is increased to 50 DEG C, other regenerated celulose fibres can dissolve, only remaining lyocell A100 and Lai Sai
Your LF is difficult to differentiate between.
4）It is insoluble that temperature is increased to only have at 70 DEG C lyocell A100, can distinguish lyocell A100 and other regenerated celluloses
Fiber.With the rise of temperature, lyocell A100 surpluses are reduced.
The selection of the temperature of experimental example 4
20 grams of anhydrous zinc chloride powder and 68 grams of anhydrous formic acids are taken, adds water quantitative to 100 grams, it is molten to prepare formic acid/zinc chloride
Liquid.Formic acid/liquor zinci chloridi is first added in tool fills in conical flask, places into standard sample, only changes temperature, carries out not equality of temperature
Under the conditions of degree, bath raio 1:100,20min, 100 times/min is vibrated, carries out standard items solubility test.As a result such as table 5：
The solubility property of regenerated celulose fibre after the temperature change of table 5
It can be seen from the data in Table 5 that at 70 DEG C, according to lyocell A100 and the difference of other Fibrinolysis performances,
Can be by lyocell A100 and other fiber separations, therefore it is 70 DEG C to select Optimal Temperature.
The selection of time of experimental example 5
20 grams of anhydrous zinc chloride powder and 68 grams of anhydrous formic acids are taken, adds water quantitative to 100 grams, it is molten to prepare formic acid/zinc chloride
Liquid.Formic acid/liquor zinci chloridi is first added in tool fills in conical flask, places into standard sample, only changes the time, when carrying out different
Between under the conditions of, bath raio 1:100,70 DEG C, 100 times/min is vibrated, carries out standard items solubility test.As a result such as table 6：
The solubility property of regenerated celulose fibre after the time change of table 6
According to data in table 6, optimal time is 20min under the conditions of 70 DEG C.
The frequency of oscillation of experimental example 6 selects
20 grams of anhydrous zinc chloride powder and 68 grams of anhydrous formic acids are taken, adds water quantitative to 100 grams, it is molten to prepare formic acid/zinc chloride
Liquid.Formic acid/liquor zinci chloridi is first added in tool fills in conical flask, places into standard sample, a frequency of oscillation changes, and carries out not
Under the conditions of frequency of oscillation, bath raio 1:100,70 DEG C, 20min, carry out standard items solubility test.As a result such as table 7：
The solubility property of regenerated celulose fibre after the change of the frequency of oscillation of table 7
According to data in upper table, it is found that influence of the frequency of oscillation to fibre identification be not notable, but frequency of oscillation is 100
During secondary/min, lyocell LF dissolves relatively complete, and viscosity is small, is more easy to differentiate, therefore selects：100 times/min.
The bath raio of experimental example 7 selects
20 grams of anhydrous zinc chloride powder and 68 grams of anhydrous formic acids are taken, adds water quantitative to 100 grams, it is molten to prepare formic acid/zinc chloride
Liquid.Formic acid/liquor zinci chloridi is first added in tool fills in conical flask, places into standard sample, only changes bath raio, 70 DEG C, vibrates
100 beats/min, 20min is vibrated, carries out standard items solubility test.Carry out the standard items solubility test under different condition.As a result such as
Under：
The solubility property of regenerated celulose fibre after the change of the bath raio of table 8
According to data in upper table, it is found that influence of the bath raio to fibre identification be not notable, but bath raio is 1:When 200, Lay
Sai Er A100 losses are larger, usually detection conventional 1:100, in order to be consistent with other detections, select bath raio 1:100 are used as this
The optimal bath raio of method.
The limit of identification of experimental example 8 (inspection range)
20 grams of anhydrous zinc chloride powder and 68 grams of anhydrous formic acids are taken, adds water quantitative to 100 grams, it is molten to prepare formic acid/zinc chloride
Liquid.Formic acid/liquor zinci chloridi is first added in tool fills in conical flask, the lyocell A100 fibers for choosing different proportion are fine with other
The mixture of dimension, carry out solubility test.The limit of identification of verification method.Sample detection result is as follows：
The qualitative test limit of identification measurement result of table 9
Above-mentioned experiment explanation, this method limit of identification is 1%, and inspection range is: 1%-100%.
Claims (4)
1. a kind of lyocell A100 discrimination method, it is characterised in that differentiate lyocell A100, bag from regenerated celulose fibre
Include following steps：
（a）Prepare formic acid/liquor zinci chloridi：18-25 grams of zinc chloride and 70 ± 2 grams of formic acid are taken, adds water quantitative to 100 grams；
（b）The regenerated celulose fibre sample of the fibers of A100 containing lyocell is added into step（a）In resulting solution, wherein sample with
Formic acid/liquor zinci chloridi mass ratio is 1:100,18-25 minutes are vibrated at 67-80 DEG C；
（c）Observation of steps（b）Dissolving result, solution is poured into the stainless steel mesh of 100 mesh, insoluble matter is Lay match during observation
You are A100.
2. discrimination method according to claim 1, it is characterised in that step（b）The frequency of the vibration is 100 beats/min
Clock.
3. discrimination method according to claim 1, it is characterised in that the zinc chloride is powdered.
4. according to the discrimination method described in claim any one of 1-3, it is characterised in that step（b）Temperature is protected after sample adds
67-72 DEG C is held, vibrates 18-25 minutes.
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