CN105115948B - A kind of discrimination method of natural indigo dyeing silk fabric - Google Patents
A kind of discrimination method of natural indigo dyeing silk fabric Download PDFInfo
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- CN105115948B CN105115948B CN201510414017.6A CN201510414017A CN105115948B CN 105115948 B CN105115948 B CN 105115948B CN 201510414017 A CN201510414017 A CN 201510414017A CN 105115948 B CN105115948 B CN 105115948B
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- CRDNMYFJWFXOCH-BUHFOSPRSA-N O=C(c1ccccc1N1)/C1=C(/c1ccccc1N1)\C1=O Chemical compound O=C(c1ccccc1N1)/C1=C(/c1ccccc1N1)\C1=O CRDNMYFJWFXOCH-BUHFOSPRSA-N 0.000 description 1
- JOTRJOWDDJFASP-UHFFFAOYSA-N O=C1c2ccccc2NC1C1Nc(cccc2)c2C1=O Chemical compound O=C1c2ccccc2NC1C1Nc(cccc2)c2C1=O JOTRJOWDDJFASP-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention discloses a kind of discrimination method of natural indigo dyeing silk fabric, comprise the following steps：(1) silk fabric is dyed using natural bipseudoindoxyl dye, obtains natural indigo dyeing silk fabric；(2) extract of natural indigo dyeing silk fabric is extracted；(3) extract obtained to step (2) carries out fluorometric investigation；By carrying out characterization test to natural indigo dyeing silk fabric extract, the emission peak of feature is shown in three-dimensional fluorescence spectrum figure according to the extract, so as to reach the purpose of the natural bipseudoindoxyl dye of quick discriminating and synthesizing indigo dyestuff, this method is simple to operate, practical effect is good, significant in the discriminating and maintenance of food development, textile dyeing and ancient textiles.
Description
Technical field
The present invention relates to chemical discriminating field, more particularly, to the discrimination method of natural indigo dyeing silk fabric.
Background technology
Natural bipseudoindoxyl dye is mainly that bluegrass plant is made by vinasse and white lime fermentation, is distributed in indigo plant, woaded blue, wood
In the plant containing indole acid composition such as indigo plant, acanthaceous indigo, mainly containing indigo and two kinds of pigments of indigo red.Synthesizing indigo is by aniline and chlorine
It is N-phenylglycine iron that acetic acid is condensed in the presence of ferric sulfate, add potassium hydroxide carry out mother liquor conversion, then with amino
Sodium, mixed alkali carry out alkali fusion generation 3- indoxyls, by air oxidation, filtering, crushing, drying and commercialization, obtain commercial dye
Indigo finished product.Compared with other natural dyes, natural indigo middle pigment composition is few, only mainly contains indigo and indigo red two
Kind pigmentary structures：
Due to comprising only a kind of indigo structure in synthesizing indigo, therefore according to natural indigo and synthesizing indigo in structure
Difference, it can be differentiated by some spectral techniques.At present, in terms of to natural indigo and synthesizing indigo dyed fabric discriminating
Study fewer, and method is limited.The discrimination method published at present in document mainly has thin-layer chromatography, oxidizing process etc., still
These methods are bigger to fabric damage, and the degree of discrimination is not high.
The content of the invention
It is an object of the invention to provide a kind of discrimination method of natural indigo dyeing silk fabric, to natural indigo dyeing
Silk fabric extract progress characterization test, the characteristic emission peak shown according to the extract in three-dimensional fluorescence spectrum figure,
So as to reach the purpose of quick discriminating；This method is simple to operate, and practical effect is good, food development, textile dyeing and
It is significant in the discriminating and maintenance of ancient textiles.
In order to solve the above-mentioned technical problem, adopt the following technical scheme that:
The discrimination method of natural indigo dyeing silk fabric, takes natural bipseudoindoxyl dye and silk fabric, its feature exists first
In including following discrimination process：
(1) indigo dyeing：Using reduction stain method, natural bipseudoindoxyl dye is dyed silk fabric, obtain day
Right indigo dyeing silk fabric；
(2) natural indigo dyeing silk fabric extract is extracted：The natural indigo dyeing silk fabrics of 1g are taken, add 15ml first
Alcoholic solution, natural indigo dyeing silk fabric is totally submerged in methanol solution；Then by natural indigo dyeing silk fabric
15~20min is extracted at 50 DEG C, extract is obtained, extract is placed in quartz colorimetric utensil；
(3) fluorometric investigation：Take extract to be placed in sepectrophotofluorometer, extract is carried out using three-dimensional fluorescence method glimmering
Optical tests, first adjust the test parameter of sepectrophotofluorometer, including exciting slit width, transmite slit width and photomultiplier transit
Pipe signal, and determine that scanning wavelength is 200~780nm；Then extract is scanned, obtains three-dimensional fluorescence spectrum figure.
After it is preferred that, the detailed process of indigo dyeing is in step (1)：(a) reduce：Determine that bath raio is 1 ︰ 50 first, then
Accurately weigh natural bipseudoindoxyl dye 5% (o.w.f), Na2S2O40.8g/l, NaOH 0.6g/l, natural bipseudoindoxyl dye is added to
In dyeing cup, and add water and mix well, Na is then added into dyeing cup2S2O4, NaOH and water, stock vatting 30min obtain transparent yellowish green
Color dye bath；(b) aoxidize：Take 2.0g silk fabrics to contaminate completely into dye bath, contaminate fully oxidized 2min after 120s, and repetition pair
Silk fabric is contaminated-aoxidized 6 times, and finally silk fabric is soaped and dried, and natural indigo dyeing silk is obtained after drying
Fabric.Dyed using oxide-reduction method, dye-uptake is high, even dyeing.
After it is preferred that, Na is added in step (a) in reduction process2S2O4Specific method with NaOH is：First added into dyeing cup
2/3 Na2S2O4, 2/3 NaOH and 1/3 water, it is 40 DEG C to control initial temperature in dyeing cup, 50 DEG C is then heated to, 50
Stock vatting 10min at DEG C；Then remaining 1/3NaOH, 1/3Na are added into dyeing cup2S2O4With 2/3 water, at 50 DEG C do
Cylinder reductase 12 0min.Na is added batch-wise2S2O4It can contribute to uniformly upper contaminate uniformly by reducing dyes into leuco compound with NaOH.
After it is preferred that, the detailed process soaped in step (b) oxidizing process is：Preparation detergent 209 is 1g/l, and sodium carbonate is
1g/l liquid of soaping, silk fabric is put into liquid of soaping, and soap 10min at 95 DEG C.The dyestuff of the not upper dye in surface is washed away,
Improve the color fastness of silk fabric.
After it is preferred that, natural indigo dyeing silk fabric extracts 20min at 50 DEG C in step (2).Under the preferred time, extraction
Take thoroughly, more extracts can be extracted.
After it is preferred that, exciting slit width is 5nm in step (3).
After it is preferred that, transmite slit width is 5nm in step (3).
After it is preferred that, photomultiplier tube signal is 350V in step (3).
Due to using above-mentioned technical proposal, having the advantages that：
The present invention is the discrimination method of natural indigo dyeing silk fabric, and natural indigo dyeing silk fabric extract is entered
Row characterization test, the characteristic emission peak shown according to the extract in three-dimensional fluorescence spectrum figure, so as to reach quick discriminating
Purpose, this method is simple to operate, and practical effect is good, in the discriminating of food development, textile dyeing and ancient textiles
With it is significant in maintenance.It is specific effective to show as：
1st, damage discriminating using micro, significantly reduce the loss of material in differentiating, avoid waste of material, cut down differentiate into
This, has broader practice market.
2nd, this method is easy to operate, and instrument is less, easy to get started, operational error occurs and causes to differentiate the probability to fail
It is low, therefore differentiate that success rate is high.
3rd, whether to there is the emission peak of feature as foundation is differentiated, identification result is intuitively clear, avoids cumbersome calculating
Process, it is practical, there is great application value.
Brief description of the drawings
The invention will be further described below in conjunction with the accompanying drawings：
Fig. 1 is the three-dimensional fluorescence spectrum figure of the extract of natural indigo dyeing silk fabric；
Fig. 2 is the three-dimensional fluorescence spectrum figure for the extract that synthesizing indigo dyes silk fabric.
EM is Emission abbreviation in wherein Fig. 1 and Fig. 2, represents launch wavelength, and EX is Excitation abbreviation, table
Show excitation wavelength.
Embodiment
The present invention on natural indigo dyeing silk fabric by extracting extract, by the extract in fluorescence spectrophotometry
Characterization test is carried out on meter, shows the emission peak of feature in three-dimensional fluorescence spectrum figure according to the extract, it is fast so as to reach
The purpose that speed differentiates.
Include following experiment material, medicine and instrument in the present invention：
Material：Silk fabric (50g/m2) and natural bipseudoindoxyl dye；
Medicine：Na2S2O4, NaOH, sodium carbonate and methanol；
Instrument：Sepectrophotofluorometer, digital constant temperature oscillator.
With reference to specific embodiment, the invention will be further described：
Embodiment
(1) indigo dyeing：Take natural bipseudoindoxyl dye and silk fabric first, using reduction stain method, dyeing and
Formula such as table 1 below：
The natural indigo dyeing silk fabric technique of table 1 and formula
(a) reduce：Determine that bath raio is 1 ︰ 50, then accurately weighs natural bipseudoindoxyl dye 5% (o.w.f), Na first2S2O4
0.8g/l, NaOH 0.6g/l, natural bipseudoindoxyl dye is added in dyeing cup, and adds a small amount of water and mix well；Then add into dyeing cup
Enter 2/3 Na2S2O4, 2/3 NaOH and 1/3 water, the amount of now dye bath is 1/3；, it is 40 to control the initial temperature in dyeing cup
DEG C, 50 DEG C are then gradually heating to, the stock vatting 10min at 50 DEG C；Then remaining 1/3NaOH, 1/ are added into dyeing cup
3Na2S2O4Water with 2/3, the stock vatting 20min at 50 DEG C, obtains transparent yellow green dye bath.
(b) aoxidize：Take 2.0g silk fabrics to contaminate completely into dye bath, fully oxidized 2min after 120s is contaminated, during dip-dye
Temperature control repeats silk fabric to be contaminated-aoxidized 6 times at 30 DEG C；After repetition dip-dye-oxidation 6 times, silk fabric is carried out
Soap：Preparation detergent 209 is 1g/l, and sodium carbonate is 1g/l liquid of soaping, and silk fabric is put into liquid of soaping, at 95 DEG C
Under soap 10min.The dyestuff of the not upper dye in surface is washed away after soaping, improves the color fastness of silk fabric.Dried after soaping, after drying
Obtain natural indigo dyeing silk fabric.
(2) natural indigo dyeing silk fabric extract is extracted：The natural indigo dyeing silk fabrics of 1g are taken, add 15ml first
Alcoholic solution, natural indigo dyeing silk fabric is totally submerged in methanol solution；Then 20min is extracted at 50 DEG C, obtained
Extract, extract is placed in quartz colorimetric utensil；
(3) fluorometric investigation：Take extract to be placed in sepectrophotofluorometer, extract is carried out using three-dimensional fluorescence method glimmering
Optical tests, the test parameter for first adjusting sepectrophotofluorometer are：Exciting slit width：5nm, transmite slit width：4nm, light
Electric multiplier tube signal：350V, and determine that scanning wavelength is 200~780nm；Then extract is scanned, is obtained such as Fig. 1 in accompanying drawing
Three-dimensional fluorescence spectrum figure,
As shown in Figure 1, there is the emission peak of feature at 495nm in the extract of natural indigo dyeing silk fabric, and glimmering
Luminous intensity is weaker, is 0.175.Because indigo red with it is indigo be in transconfiguration, indigo red stability is better than indigo, is reducing
The structure of indigo red will not change in oxidizing process, and indigo red has less fluorescence property, cause natural indigo dye
Certain fluorescence property is presented in the extract of color silk fabric, i.e., occurs the emission peak of feature at 495nm.
Reference examples
(1) indigo dyeing：Using indigo dyeing method in embodiment, will be contaminated on synthesizing indigo dyestuff into silk fabric,
Obtain synthesizing indigo dyeing silk fabric
(2) synthesizing indigo dyeing silk fabric extract is extracted：Take 1g synthesizing indigos to dye silk fabric, add 15ml first
Alcoholic solution, synthesizing indigo dyeing silk fabric is totally submerged in methanol solution；Then 20min is extracted at 50 DEG C, obtained
Extract, extract is placed in quartz colorimetric utensil；
(3) fluorometric investigation：Take extract to be placed in sepectrophotofluorometer, extract is carried out using three-dimensional fluorescence method glimmering
Optical tests, the test parameter for first adjusting sepectrophotofluorometer are：Exciting slit width：5nm, transmite slit width：4nm, light
Electric multiplier tube signal：350V, and determine that scanning wavelength is 200~780nm；Then extract is scanned, is obtained such as Fig. 2 in accompanying drawing
Three-dimensional fluorescence spectrum figure.
There is not the hair of feature in the range of 200~780nm in synthesizing indigo dyeing silk fabric extract as shown in Figure 2
Penetrate peak, this be primarily due to synthesizing indigo include it is indigo and indigo white, it is indigo white not have fluorescence property, during reduction-oxidation
It is indigo be reduced into it is indigo white, this cause synthesizing indigo dyeing silk fabric extract certain fluorescence property is not presented, i.e.,
There is no the emission peak of feature.It is wherein indigo that to be converted into indigo white principle as follows：
By comparative example and reference examples, it is indigo and it is indigo white there is no fluorescence property, indigo red has the glimmering of some strength
Optical property, this causes the extract of natural indigo dyeing silk fabric to dye the extract of silk fabric in three-dimensional with synthesizing indigo
Occur certain fluorescent differences in fluorescence spectra, can be as the natural indigo and discriminating foundation of synthesizing indigo.
The specific embodiment of the present invention is these are only, but the technical characteristic of the present invention is not limited thereto.It is any with this hair
Based on bright, to solve essentially identical technical problem, essentially identical technique effect is realized, made ground simple change, etc.
With replacement or modification etc., all it is covered by among protection scope of the present invention.
Claims (7)
1. a kind of discrimination method of natural indigo dyeing silk fabric, takes natural bipseudoindoxyl dye and silk fabric, its feature first
It is to include following discrimination process：
(1) indigo dyeing：(a) reduce：Determine that bath raio is 1 ︰ 50, then accurately weighs natural bipseudoindoxyl dye 5% first
(o.w.f)、Na2S2O40.8g/l, NaOH0.6g/l, natural bipseudoindoxyl dye is added in dyeing cup, and adds water and mix well, then
Na2S2O4, NaOH are added into dyeing cup and water, stock vatting 30min obtain transparent yellow green dye bath；(b) aoxidize：Take 2.0g silkworms
Silk fabrics is contaminated into dye bath completely, contaminates fully oxidized 2min after 120s, and repeats silk fabric to be contaminated-aoxidized 6 times, most
Silk fabric is soaped and dried afterwards, natural indigo dyeing silk fabric is obtained after drying；
(2) natural indigo dyeing silk fabric extract is extracted：The natural indigo dyeing silk fabrics of 1g are taken, it is molten to add 15ml methanol
Liquid, natural indigo dyeing silk fabric is totally submerged in methanol solution；Then by natural indigo dyeing silk fabric 50
15~20min is extracted at DEG C, extract is obtained, extract is placed in quartz colorimetric utensil；
(3) fluorometric investigation：Take extract to be placed in sepectrophotofluorometer, fluorescence survey is carried out to extract using three-dimensional fluorescence method
Examination, first adjust the test parameter of sepectrophotofluorometer, including exciting slit width, transmite slit width and photomultiplier letter
Number, and determine that scanning wavelength is 200nm~780nm；Then extract is scanned, obtains three-dimensional fluorescence spectrum figure.
A kind of 2. discrimination method of natural indigo dyeing silk fabric according to claim 1, it is characterised in that：The step
(a) addition Na2S2O4 and NaOH specific method is in reduction process in：2/3 Na2S is first added into dyeing cup2O4, 2/3
NaOH and 1/3 water, it is 40 DEG C to control the initial temperature in dyeing cup, then heats to 50 DEG C, the stock vatting at 50 DEG C
10min；Then remaining 1/3NaOH, 1/3Na are added into dyeing cup2S2O4With 2/3 water, the stock vatting 20min at 50 DEG C.
A kind of 3. discrimination method of natural indigo dyeing silk fabric according to claim 1, it is characterised in that：The step
(b) detailed process soaped in oxidizing process is：Preparation detergent 209 is 1g/l, and sodium carbonate is 1g/l liquid of soaping, by silk
Fabric is put into liquid of soaping, and soap 10min at 95 DEG C.
A kind of 4. discrimination method of natural indigo dyeing silk fabric according to claim 1, it is characterised in that：The step
(2) natural indigo dyeing silk fabric extracts 20min at 50 DEG C in.
A kind of 5. discrimination method of natural indigo dyeing silk fabric according to claim 1, it is characterised in that：The step
(3) exciting slit width is 5nm in.
A kind of 6. discrimination method of natural indigo dyeing silk fabric according to claim 1, it is characterised in that：The step
(3) transmite slit width is 5nm in.
A kind of 7. discrimination method of natural indigo dyeing silk fabric according to claim 1, it is characterised in that：The step
(3) photomultiplier tube signal is 350V in.
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| CN105628817A (en) * | 2015-12-29 | 2016-06-01 | 武汉纺织大学 | Method for distinguishing natural indigo blue and synthetic indigo blue dyed fabrics |
| CN109900647B (en) * | 2019-03-04 | 2022-04-05 | 青岛大学 | Quick chromatographic identification method for plant-dyed cotton fabric and chemical-dyed cotton fabric |
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| WO2012135622A1 (en) * | 2011-03-31 | 2012-10-04 | Celanese International Corporation | Disperse dyeing of textile fibers |
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