CN104764736A - Method for identifying lyocell A100 and application of method - Google Patents
Method for identifying lyocell A100 and application of method Download PDFInfo
- Publication number
- CN104764736A CN104764736A CN201510143405.5A CN201510143405A CN104764736A CN 104764736 A CN104764736 A CN 104764736A CN 201510143405 A CN201510143405 A CN 201510143405A CN 104764736 A CN104764736 A CN 104764736A
- Authority
- CN
- China
- Prior art keywords
- lyocell
- formic acid
- discrimination method
- regenerated celulose
- liquor zinci
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
The invention relates to a method for identifying lyocell A100 in regenerated cellulose fiber. The method comprises the following steps: dissolving a sample containing lyocell A100 in a formic acid/zinc chloride solution, observing an insoluble substance after the dissolution reaction, and qualitatively detecting whether the sample contains lyocell A100. The invention further provides application of the method in detection of lyocell A100. The method can be used for quickly and accurately identifying lyocell A100 in other regenerated cellulose fiber, is a qualitative identification method with high feasibility and meanwhile lays a foundation for quantitative analysis of lyocell A100.
Description
Technical field
The invention belongs to fibre identification technical field, be specifically related to the method differentiating lyocell A100 from regenerated celulose fibre, relate to simultaneously its lyocell A100 differentiate in application.
Background technology
Due to the minimizing in arable land and the day by day exhausted of petroleum resources, the output of natural fiber, synthon is subject to increasing restriction, and people, while attention textile environmental-protecting performance, more and more pay attention to the development and utilization of regenerated celulose fibre.Regenerated celulose fibre belongs to native cellulose regenerated fibre, its structure composition is quite similar with cotton fiber, but performance excellent as the silk but having cotton fiber not possess, regenerated celulose fibre is a kind of function admirable " environmental protection " fiber, and its waste and old gurry can natural degradation.Regenerated celulose fibre is the direction of future development, is the effective way solving natural resources shortage.
Regenerated celulose fibre refers to the native cellulose class raw material of, degradable renewable by cotton linter, straw, beech, eucalyptus, bamboo etc., environmental protection, through the tencel that can be used in weaving that special process is produced, the basic composition of these fibers is cellulose IIs.Mainly contain: the common viscose fiber that 20 beginnings of the century emerged, the koplon of the fifties, CUP; The Modal fibre in the Lenzin company later stage eighties; The Lyocell fibers that commercialization nineties performance is more excellent; The bamboo pulp fiber etc. of last century Mo China's invention.Their general character: manufacture raw material (base material) character close---native cellulose; Technique is close---and cellulose dissolution is spinning again; Molecular structure is similar---large molecules fibrin II; Chemical property-the solubility property of fiber itself is similar.Their difference: only slightly different, the physical property of molecular weight is slightly distinguished, but wearing comfort has a great difference, and price has notable difference.Due to so many similar, making to carry out qualitative and quantitative analysis accurately to them becomes one of difficult problem that in current world wide, textile fiber composition detection field is generally acknowledged.
Fiber content detection is the project of domestic and international technical regulation compulsory test, and in recent years, the consumption fraud problems that textile fibres mark composition and reality do not conform to is very general, accounts for textile product nonconformance object more than 80%.Particularly, the appearance of tencel in recent years, because these fibrous raw material price variances are larger, these fraud problems of prevention and control are in the urgent need to developing new detection technique, the carrying out done one's utmost in the discriminating coherent detection field of this fiber is always studied, but all there is not yet correlative regeneration fiber blend product composition at home and abroad to detect, the report of effective and feasible detection method.Along with scientific-technical progress, the kind of regenerated celulose fibre is also in continuous increase, and it is differentiated, detection technique is badly in need of haveing breakthrough.The discriminating of regenerated celulose fibre such as presented hereinbefore and quantitative test just do not have effective method and detect foundation reliably, thus occur mixing the spurious with the genuine, the problem of dolus malus consumer is very general, therefore, invent a kind of method differentiating Lyocell fibers from regenerated celulose fibre very urgent, have extremely important realistic meaning.What current regenerated celulose fibre had used in a large number has: common viscose fiber, Modal, lyocell, bamboo fibre etc.
Lyocell fibers is divided into lyocell A100, lyocell LF, lyocell G100 tri-kinds according to its production technology difference, but in actual application, all specialize the kind of lyocell during cotton mill buying raw material, and be only marked as Lyocell fibers after manufacturing clothes.Because the character of three kinds of lyocells is similar, effective differentiation is not enough to current classical discrimination method, chemical property again due to three kinds of lyocells is seemingly different, cause in testing process, there will be a problem: the product of the Lyocell fibers indicated equally and some fiber blend, when doing fiber content and detecting, detection data are unstable, main cause is exactly the difference accurately can not differentiating that lyocell A100, lyocell LF, lyocell G100 are of the same clan, the quantitative analysis method of more do not know where to begin lyocell A100 and other regenerated celulose fibres.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of simple, the highly sensitive method differentiating lyocell A100 from regenerated celulose fibre of flow process, provides it to apply simultaneously.
The technical scheme that the present invention solves the employing of its technical matters is: the discrimination method of a kind of lyocell A100, differentiates lyocell A100, comprise the following steps from regenerated celulose fibre:
(a) preparation formic acid/liquor zinci chloridi: get 18-25 gram of zinc chloride and (70 ± 2) gram formic acid, add water quantitatively to 100 grams;
B regenerated celulose fibre sample containing lyocell A100 fiber adds in step (a) gained solution by (), vibrate 18-25 minute at 67-80 DEG C;
C () observes the dissolving result of step (b), insolubles is lyocell A100.
Preferably, sample and formic acid/liquor zinci chloridi mass ratio are 1:100.
Preferably, the frequency of the described vibration of step (b) is 100 beats/min.
Preferably, described zinc chloride is Powdered.
Preferably, solution is poured into 100 object stainless steel mesh when step (c) is observed.
Preferably, step (b) sample adds rear temperature and keeps 67-72 DEG C, vibration 18-25 minute.
The present invention provides described discrimination method differentiating the application in lyocell A100 simultaneously.
Good effect of the present invention is, the qualitative identification method providing a kind of lyocell A100 of the invention, adopt method of the present invention lyocell A100 can be identified from other regenerated celulose fibres, required preparation of reagents is simple, under reaction time provided by the invention and temperature, discrimination threshold is high, and exploitativeness is strong.
The invention provides formic acid/liquor zinci chloridi and differentiate that the method for fiber is differentiating the application in lyocell A100, formic acid in GB/T2910.6-2009/zinc chloride differentiates cotton and Lyocell fibers, therefore, Lyocell fibers is dissolved in the common practise that the formic acid/liquor zinci chloridi in standard is those skilled in the art.But the present inventor is in concrete operations, it is unexpected that discovery lyocell A100 be insoluble to formic acid/liquor zinci chloridi under certain condition, the dissolubility of lyocell A100 and regenerated celulose fibre have nuance at the dissolution conditions of formic acid/liquor zinci chloridi, through great many of experiments with repeatedly investigate, finally determine the top condition that it differentiates lyocell A100, provide the application of discrimination method in lyocell A100 differentiates in a creative way.
Embodiment
For enabling above-mentioned purpose of the present invention, feature and advantage become apparent more, below the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
In technical solution of the present invention, prepare formic acid/liquor zinci chloridi with 68 grams of anhydrous formic acids and 80 gram of 88% formic acid, the every testing result of gained all has consistance.
embodiment 1 differentiates lyocell A100 from regenerated celulose fibre
Embodiment 1 concrete grammar is: get 18-25 gram of anhydrous chlorides of rase zinc powder and 68 grams of anhydrous formic acids, adds water quantitatively to 100 grams, preparation formic acid/liquor zinci chloridi.In tool plug Erlenmeyer flask, first add formic acid/liquor zinci chloridi, then put into measuring samples, described sample and formic acid/liquor zinci chloridi mass ratio are 1:100, cover bottle stopper, vibrate 20min at 70 DEG C, pours in 100 object stainless steel mesh, look into and see if there is residue.Residue insolubles is lyocell A100.
Embodiment 1 measuring samples is 6 groups, and sample all adopts known fiber to be obtained by mixing, and the concrete composition of sample is in table 1; After discrimination method reaction, the quality of the anhydrous zinc chloride selected during 6 groups of sample dissolution and identification result are in table 1.Visible, the testing result of the discrimination method of the present embodiment is consistent with reality, and accuracy rate is higher.
The composition of table 1 embodiment 1 each sample, the amount detecting use zinc chloride and testing result
Note: " √ " represents containing this composition.
experimental example 1 reagent is selected
Generally differentiate that the primary solvent of cellulose fibre has sulfuric acid, hydrochloric acid, nitric acid, copper ammon solution by dissolution method, in quantitative test, conventional sulfuric acid, formic acid liquor zinci chloridi, also use sodium zincate solution, NaOH/thiocarbamide/urea liquid etc. sometimes.With 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, and test under the bath raio shown in table 2, temperature, time, oscillation frequency, result is as table 2.
The dissolubility of the various regenerated celulose fibre of table 2 in reagent
conclusion:
1) formic acid/zinc chloride is optimum reagent lyocell A100 and fast, the sensitive difference of other regenerated celulose fibres come.
2) lyocell A100 and lyocell LF, lyocell G100 cannot distinguish and come by NaOH/thiocarbamide/urea reagent.
3) sulfuric acid, hydrochloric acid, nitric acid, copper ammon solution four kinds of solution are the reagent of the discriminating cellulose fiber Wesy that FZ/T 01057.3-2007 lists, but lyocell A100 and the qualitative difference of other regenerated celulose fibres can not come by they.
Therefore, the optimal conditions that when below testing primary study using formic acid/zinc chloride as solvent, lyocell A100 and other regenerated celulose fibres are differentiated is selected.
the selection of experimental example 2 formic acid/zinc chloride reagent ratio range and optimal proportion
At 70 DEG C, according to table 3 reagent preparation, solubilizing reaction time 20min, the solubility property of each regenerated celulose fibre is in table 3.
The solubility property of each regenerated celulose fibre under table 3 different reagent proportioning
conclusion:
1) regenerated celulose fibres such as viscose glue, Modal, bamboo fibre can all dissolve by certain density formic acid/zinc chloride.
2) when in formic acid, zinc oxide concentration is too low, three kinds of Lyocell fibers can not be distinguished, only have when zinc chloride reaches certain concentration, lyocell LF and lyocell G100 could dissolve completely, residue lyocell A100.
3) differentiate that in formic acid/zinc chloride that lyocell A100 uses, zinc chloride content at least should be 20g/100g, consider the principle of environmental protection and easy operation, the compound method of formic acid/zinc chloride is that 20g anhydrous zinc chloride (massfraction > 98%) joins in 88% formic acid of 80g.
experimental example 3 temperature-time scope is selected
Get 20 grams of anhydrous chlorides of rase zinc powders and 68 grams of anhydrous formic acids, add water quantitatively to 100 grams, preparation formic acid/liquor zinci chloridi.In tool plug Erlenmeyer flask, first add formic acid/liquor zinci chloridi, then put into measuring samples, described sample and formic acid/liquor zinci chloridi mass ratio are 1:100, cover bottle stopper, vibrate under temperature and time shown in table 4, pour in 100 object stainless steel mesh, look into and see if there is residue, the results are shown in Table 4.
The solubility property of each regenerated celulose fibre under the temperature and time that table 4 is different
conclusion:
1) when temperature is lower, Lyocell fibers is all comparatively stable, not soluble, therefore viscose glue, Modal and bamboo fibre and Lyocell fibers can be distinguished.
2) along with the rising of temperature, the rate of dissolution of viscose glue, Modal and bamboo fibre is accelerated, and can dissolve within a short period of time completely, but lyocell A100, lyocell G100 and lyocell LF are difficult to distinguish.
3) when temperature is increased to 50 DEG C, other regenerated celulose fibres can dissolve, and only remain lyocell A100 and lyocell LF and are difficult to distinguish.
4) only there is lyocell A100 insoluble when temperature is increased to 70 DEG C, lyocell A100 and other regenerated celulose fibres can be distinguished.Along with the rising of temperature, lyocell A100 surplus reduces.
the selection of experimental example 4 temperature
Get 20 grams of anhydrous chlorides of rase zinc powders and 68 grams of anhydrous formic acids, add water quantitatively to 100 grams, preparation formic acid/liquor zinci chloridi.In tool plug Erlenmeyer flask, first add formic acid/liquor zinci chloridi, then put into standard model, only change temperature, under carrying out condition of different temperatures, bath raio 1:100,20min, vibration 100 times/min, carries out standard items solubility test.Result is as table 5:
The solubility property of the regenerated celulose fibre after table 5 temperature variation
Data as can be seen from table 5,70 DEG C time, different according to lyocell A100 and other Fibrinolysis performances, can, by lyocell A100 and other fiber separation, therefore select Optimal Temperature to be 70 DEG C.
experimental example 5 selection of time
Get 20 grams of anhydrous chlorides of rase zinc powders and 68 grams of anhydrous formic acids, add water quantitatively to 100 grams, preparation formic acid/liquor zinci chloridi.In tool plug Erlenmeyer flask, first add formic acid/liquor zinci chloridi, then put into standard model, only change the time, under carrying out different time condition, bath raio 1:100,70 DEG C, vibration 100 times/min, carries out standard items solubility test.Result is as table 6:
The solubility property of the regenerated celulose fibre after table 6 time variations
According to data in table 6, under 70 DEG C of conditions, optimal time is 20min.
experimental example 6 oscillation frequency is selected
Get 20 grams of anhydrous chlorides of rase zinc powders and 68 grams of anhydrous formic acids, add water quantitatively to 100 grams, preparation formic acid/liquor zinci chloridi.In tool plug Erlenmeyer flask, first add formic acid/liquor zinci chloridi, then put into standard model, an oscillation frequency changes, and under carrying out different oscillation frequency condition, bath raio 1:100,70 DEG C, 20min, carries out standard items solubility test.Result is as table 7:
The solubility property of the regenerated celulose fibre after the change of table 7 oscillation frequency
According to data in above table, find that oscillation frequency is not remarkable on the impact of fibre identification, but oscillation frequency is when 100 times/min, it is comparatively complete that lyocell LF dissolves, and viscosity is little, more easily differentiates, therefore selects: 100 times/min.
experimental example 7 bath raio is selected
Get 20 grams of anhydrous chlorides of rase zinc powders and 68 grams of anhydrous formic acids, add water quantitatively to 100 grams, preparation formic acid/liquor zinci chloridi.In tool plug Erlenmeyer flask, first add formic acid/liquor zinci chloridi, then put into standard model, only change bath raio, 70 DEG C, vibrate 100 beats/min, vibration 20min, carries out standard items solubility test.Carry out the standard items solubility test under different condition.Result is as follows:
The solubility property of regenerated celulose fibre after the change of table 8 bath raio
According to data in above table, find that bath raio is not remarkable on the impact of fibre identification, but bath raio is when 1:200, lyocell A100 loses larger, detecting conventional 1:100 at ordinary times, being consistent to detect with other, select bath raio 1:100 as the optimum bath raio of this method.
experimental example 8 limit of identification (inspection range)
Get 20 grams of anhydrous chlorides of rase zinc powders and 68 grams of anhydrous formic acids, add water quantitatively to 100 grams, preparation formic acid/liquor zinci chloridi.In tool plug Erlenmeyer flask, first add formic acid/liquor zinci chloridi, choose the lyocell A100 fiber of different proportion and the potpourri of other fibers, carry out solubility test.The limit of identification of verification method.Sample detection result is as follows:
Table 9 qualitative test limit of identification measurement result
Above-mentioned test illustrates, the method limit of identification is 1%, and inspection range is: 1%-100%.
Claims (7)
1. a discrimination method of lyocell A100, is characterized in that, differentiates lyocell A100, comprise the following steps from regenerated celulose fibre:
(a) preparation formic acid/liquor zinci chloridi: get 18-25 gram of zinc chloride and (70 ± 2) gram formic acid, add water quantitatively to 100 grams;
B regenerated celulose fibre sample containing lyocell A100 fiber adds in step (a) gained solution by (), vibrate 18-25 minute at 67-80 DEG C;
C () observes the dissolving result of step (b), insolubles is lyocell A100.
2. discrimination method according to claim 1, is characterized in that, sample and formic acid/liquor zinci chloridi mass ratio are 1:100.
3. discrimination method according to claim 1, is characterized in that, the frequency of the described vibration of step (b) is 100 beats/min.
4. discrimination method according to claim 1, is characterized in that, described zinc chloride is Powdered.
5. discrimination method according to claim 1, is characterized in that, solution is poured into 100 object stainless steel mesh when step (c) is observed.
6. the discrimination method according to any one of claim 1-5, is characterized in that, step (b) sample adds rear temperature and keeps 67-72 DEG C, vibration 18-25 minute.
7. discrimination method described in any one of claim 1-6 is differentiating the application in lyocell A100.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510143405.5A CN104764736B (en) | 2015-03-30 | 2015-03-30 | Lyocell A100 discrimination method and its application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510143405.5A CN104764736B (en) | 2015-03-30 | 2015-03-30 | Lyocell A100 discrimination method and its application |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104764736A true CN104764736A (en) | 2015-07-08 |
| CN104764736B CN104764736B (en) | 2018-01-12 |
Family
ID=53646700
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510143405.5A Expired - Fee Related CN104764736B (en) | 2015-03-30 | 2015-03-30 | Lyocell A100 discrimination method and its application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104764736B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111982738A (en) * | 2020-07-22 | 2020-11-24 | 石家庄海关技术中心 | Quantitative analysis method of cross-linked lyocell fibers and viscose fibers |
| US11866519B2 (en) | 2018-09-18 | 2024-01-09 | Wool Research Organisation Of New Zealand Incorporated | Cellulose-containing materials |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004344041A (en) * | 2003-05-21 | 2004-12-09 | Asahi Kasei Chemicals Corp | Method for quantitatively analyzing water-insoluble cellulose |
| CN1940525A (en) * | 2006-09-27 | 2007-04-04 | 茅明华 | Quantitative chemcial analysis for Laishuer and cotton two-component blend fibre |
| CN102159764A (en) * | 2008-09-22 | 2011-08-17 | 连津格股份公司 | Use of lyocell fibers and items comprising lyocell fibers |
| US20140185032A1 (en) * | 2012-12-28 | 2014-07-03 | Hyundai Motor Company | Method for measuring fiber content of polyethyleneterephthalate and polytrimethyleneterephthalate fibers |
-
2015
- 2015-03-30 CN CN201510143405.5A patent/CN104764736B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004344041A (en) * | 2003-05-21 | 2004-12-09 | Asahi Kasei Chemicals Corp | Method for quantitatively analyzing water-insoluble cellulose |
| CN1940525A (en) * | 2006-09-27 | 2007-04-04 | 茅明华 | Quantitative chemcial analysis for Laishuer and cotton two-component blend fibre |
| CN102159764A (en) * | 2008-09-22 | 2011-08-17 | 连津格股份公司 | Use of lyocell fibers and items comprising lyocell fibers |
| US20140185032A1 (en) * | 2012-12-28 | 2014-07-03 | Hyundai Motor Company | Method for measuring fiber content of polyethyleneterephthalate and polytrimethyleneterephthalate fibers |
Non-Patent Citations (2)
| Title |
|---|
| 中华人民共和国国家质量监督检验检疫总局 等: "《中华人民共和国国家标准》", 15 June 2009 * |
| 陈扬: "纺织品--甲酸-氯化锌溶解法的时间与浓度控制", 《上海毛麻科技》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11866519B2 (en) | 2018-09-18 | 2024-01-09 | Wool Research Organisation Of New Zealand Incorporated | Cellulose-containing materials |
| CN111982738A (en) * | 2020-07-22 | 2020-11-24 | 石家庄海关技术中心 | Quantitative analysis method of cross-linked lyocell fibers and viscose fibers |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104764736B (en) | 2018-01-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104764671B (en) | The quantitative analysis method of lyocell A100 in the new application and composite fibre of formic acid/liquor zinci chloridi | |
| CN101260569B (en) | Regenerated cellulose viscose fiber and its preparing process | |
| CN101407550A (en) | Cellulose acetate made from raw material hemp dissolving pulp, preparation and use thereof | |
| CN104764736A (en) | Method for identifying lyocell A100 and application of method | |
| CN104914001B (en) | Application and its analysis method of the formic acid/liquor zinci chloridi in composite fibre in lyocell A100 quantitative analyses | |
| CN107245161A (en) | A kind of method of the mechanically decoupled waste and old polyester cotton of sulfuric acid | |
| CN100498281C (en) | Quantitative chemcial analysis for Laishuer and cotton two-component blend fibre | |
| CN106087088A (en) | The preparation method of regenerated celulose fibre | |
| CN104764872A (en) | Method for identifying lyocell and application of method | |
| CN101231224A (en) | Method for quantitative analysis of bicomponent fibre textile | |
| Määttänen et al. | Pre-treatments of pre-consumer cotton-based textile waste for production of textile fibres in the cold NaOH (aq) and cellulose carbamate processes | |
| CN102558571A (en) | Method for preparing alkali lignin by using corncob residues | |
| WO2022100052A1 (en) | Anti-counterfeiting modal fiber, preparation method and anti-counterfeiting method | |
| CN102426147A (en) | Method for distinguishing Lyocell bamboo fiber in blending product | |
| CN101655486B (en) | Method for detecting f.CaO influencing the utilization of stabilization of steel slag | |
| CN104931322B (en) | A kind of quantitative analysis method of cotton and viscose blend fabric | |
| CN101470064A (en) | Cotton and silk fiber blended product content analysis method | |
| CN109402757B (en) | Preparation method of anti-electromagnetic radiation lyocell fiber | |
| CN104122164A (en) | Quantitative determination method for fiber content of viloft fiber and polyester fiber blended textiles | |
| CN105647256A (en) | Waterproof flame-retardant and acid-base-resisting coating for fabric | |
| CN105334136A (en) | Fiber content quantitative chemical analysis method for polyester and spandex products | |
| CN102323326B (en) | Supervision and validation method of textile fiber industry supply chain | |
| CN107063917A (en) | A kind of method for determining cellulose fiber content in the natural or two-component mixture of regenerated celulose fibre and polyester fiber | |
| KR101185889B1 (en) | Method for quantitative analysis of cellulose fiber mixtures of textiles by chemical carbonization | |
| CN106368679A (en) | Microelement tracer agent used for offshore oilfield and use method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20180112 |