CN105115948A - Discriminating method of natural indigo dyed silk fabric - Google Patents
Discriminating method of natural indigo dyed silk fabric Download PDFInfo
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- CN105115948A CN105115948A CN201510414017.6A CN201510414017A CN105115948A CN 105115948 A CN105115948 A CN 105115948A CN 201510414017 A CN201510414017 A CN 201510414017A CN 105115948 A CN105115948 A CN 105115948A
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- indigo dyeing
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Abstract
The invention discloses a discriminating method of a natural indigo dyed silk fabric. The method comprises the following steps: 1, dyeing a silk fabric by adopting a natural indigo dye to obtain the natural indigo dyed silk fabric; 2, extracting the extract liquid of the natural indigo dyed silk fabric; and 3, carrying out fluorescence test on the extract liquid obtained in step 2. Characterization test of the extract liquid of the natural indigo dyed silk fabric is carried out, so the purpose of rapid discrimination of the natural indigo dye and a synthesized indigo dye is achieved according to characteristic emission peaks of the extraction liquid in a three dimensional fluorescence spectrogram. The method has the advantages of simple operation, good practical use effect, and great significance to food exploitation, fabric dyeing, and discrimination and maintenance of ancient textiles.
Description
Technical field
The present invention relates to chemical discriminating field, especially relate to the discrimination method of natural indigo dyeing silk fabric.
Background technology
Natural bipseudoindoxyl dye mainly bluegrass plant is obtained by vinasse and white lime fermentation, is distributed in indigo plant, woaded blue, wood indigo plant, acanthaceous indigo etc. containing in the plant of IA composition, main containing indigo and indigo red two kinds of pigments.By aniline and chloroacetic acid, condensation under iron sulfate exists is N-phenylglycine iron to synthesizing indigo, add potassium hydroxide again and carry out mother liquor conversion, then carry out alkali fusion generate 3-indoxyl with Sodamide, mixed alkali, by air oxidation, filtration, pulverizing, drying and commercialization, obtain the indigo finished product of commercial dye.Compared with other natural dyes, natural indigo middle pigment composition is few, only main containing indigo and indigo red two kinds of pigmentary structures:
Due in synthesizing indigo only containing indigo a kind of structure, therefore according to natural indigo with synthesizing indigo difference structurally, can be differentiated by some spectral techniques.At present, to natural indigo fewer with the research of synthesizing indigo dyed fabric discriminating aspect, and method is limited.The discrimination method published in current document mainly contains thin-layer chromatography, oxidizing process etc., but these methods are larger to fabric damage, and the degree of discrimination is not high.
Summary of the invention
The object of the present invention is to provide a kind of discrimination method of natural indigo dyeing silk fabric, characterization test is carried out to natural indigo dyeing silk fabric extract, according to the characteristic emission peak that this extract shows in three-dimensional fluorescence spectrum figure, thus reach the object differentiated fast; The method is simple to operate, and practical effect is good, in the discriminating of food development, textile dyeing and ancient textiles and significant in safeguarding.
In order to solve the problems of the technologies described above, adopt following technical scheme:
The discrimination method of natural indigo dyeing silk fabric, first gets natural bipseudoindoxyl dye and silk fabric, it is characterized in that comprising following discrimination process:
(1) indigo dyeing: adopt reduction stain method, natural bipseudoindoxyl dye is dyeed to silk fabric, obtains natural indigo dyeing silk fabric;
(2) natural indigo dyeing silk fabric extract is extracted: get the natural indigo dyeing silk fabric of 1g, add 15ml methanol solution, be immersed in completely in methanol solution by natural indigo dyeing silk fabric; Then natural indigo dyeing silk fabric is extracted 15 ~ 20min at 50 DEG C, be extracted liquid, extract is placed in quartz colorimetric utensil;
(3) fluorometric investigation: get extract and be placed in fluorospectrophotometer, three-dimensional fluorescence method is adopted to carry out fluorometric investigation to extract, first regulate the test parameter of fluorospectrophotometer, comprise and excite slit width, transmitting slit width and photomultiplier tube signal, and determine that scanning wavelength is 200 ~ 780nm; Then scan extract, obtain three-dimensional fluorescence spectrum figure.
Preferably, in step (1), the detailed process of indigo dyeing is: (a) reduces: first determine that bath raio is 1 ︰ 50, then accurately take natural bipseudoindoxyl dye 5% (o.w.f), Na
2s
2o
40.8g/l, NaOH0.6g/l, join natural bipseudoindoxyl dye in dye cup, and add water and mix well, and then in dye cup, adds Na
2s
2o
4, NaOH and water, stock vatting 30min obtains the green dye bath of transparent yellow; B () is oxidized: get 2.0g silk fabric and contaminate in dye bath completely, fully oxidized 2min after dip-dye 120s, and repeats to contaminate-be oxidized 6 times to silk fabric, finally soaps to silk fabric and dries, drying the natural indigo dyeing silk fabric of rear acquisition.Employing oxide-reduction method dyes, and dye-uptake is high, even dyeing.
Preferably, in step (a), in reduction process, add Na
2s
2o
4with the concrete grammar of NaOH be: first to contaminating in cup the Na adding 2/3
2s
2o
4, the NaOH of 2/3 and the water of 1/3, the initial temperature controlled in dye cup is 40 DEG C, is then warming up to 50 DEG C, stock vatting 10min at 50 DEG C; Then in dye cup, remaining 1/3NaOH, 1/3Na is added
2s
2o
4with 2/3 water, stock vatting 20min at 50 DEG C.Add Na in batches
2s
2o
4uniformly reducing dyes can be become leuco compound with NaOH, contribute to evenly upper dye.
Preferably, the detailed process of soaping in step (b) oxidizing process is: preparation detergent 209 is 1g/l, and sodium carbonate is the liquid of soaping of 1g/l, is put into by silk fabric and soaps in liquid, and soap 10min at 95 DEG C.Wash away the dyestuff of the not upper dye in surface, improve the colour fastness of silk fabric.
Preferably, in step (2), natural indigo dyeing silk fabric extracts 20min at 50 DEG C.Under this preferred time, extraction thoroughly, can extract more extract.
Preferably, slit width in step (3), is excited to be 5nm.
Preferably, launching slit width in step (3) is 5nm.
Preferably, in step (3), photomultiplier tube signal is 350V.
Owing to adopting technique scheme, there is following beneficial effect:
The present invention is the discrimination method of natural indigo dyeing silk fabric, characterization test is carried out to natural indigo dyeing silk fabric extract, according to the characteristic emission peak that this extract shows in three-dimensional fluorescence spectrum figure, thus reach the object differentiated fast, the method is simple to operate, practical effect is good, in the discriminating of food development, textile dyeing and ancient textiles and significant in safeguarding.It is specifically effective shows as:
1, adopt trace to damage discriminating, significantly reduce the loss of material in differentiating, avoid waste of material, cut down and differentiate cost, there is more wide application market.
2, the method is easy and simple to handle, and instrument is less, easy left-hand seat, occurs misoperation and causes differentiating that failed probability is low, therefore differentiates that success ratio is high.
3, whether to occur that the emission peak of feature is for differentiating foundation, identification result is intuitively clear, avoids loaded down with trivial details computation process, practical, has great using value.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the invention will be further described:
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 of the extract of synthesizing indigo dyeing silk fabric.
Wherein in Fig. 1 and Fig. 2, EM is the abbreviation of Emission, and represent emission wavelength, EX is the abbreviation of Excitation, represents excitation wavelength.
Embodiment
This extract, by extracting extract on natural indigo dyeing silk fabric, fluorospectrophotometer is carried out characterization test, shows the emission peak of feature according to this extract in three-dimensional fluorescence spectrum figure by the present invention, thus reaches the object differentiated fast.
Following experiment material, medicine and instrument is included in the present invention:
Material: silk fabric (50g/m
2) and natural bipseudoindoxyl dye;
Medicine: Na
2s
2o
4, NaOH, sodium carbonate and methyl alcohol;
Instrument: fluorospectrophotometer, digital constant temperature oscillator.
Below in conjunction with specific embodiment, the invention will be further described:
Embodiment
(1) indigo dyeing: first get natural bipseudoindoxyl dye and silk fabric, adopts reduction stain method, and dyeing and formula are as following table 1:
Table 1 natural indigo dyeing silk fabric technique and formula
A () is reduced: first determine that bath raio is 1 ︰ 50, then accurately take natural bipseudoindoxyl dye 5% (o.w.f), Na
2s
2o
40.8g/l, NaOH0.6g/l, join natural bipseudoindoxyl dye in dye cup, and add a small amount of water and mix well; Then in dye cup, add the Na of 2/3
2s
2o
4, the NaOH of 2/3 and the water of 1/3, the amount of now dye bath is 1/3; , the initial temperature controlled in dye cup is 40 DEG C, is then warming up to 50 DEG C gradually, stock vatting 10min at 50 DEG C; Then in dye cup, remaining 1/3NaOH, 1/3Na is added
2s
2o
4with the water of 2/3, stock vatting 20min at 50 DEG C, obtains the green dye bath of transparent yellow.
B () is oxidized: get 2.0g silk fabric and contaminate in dye bath completely, fully oxidized 2min after dip-dye 120s, and during dip-dye, temperature controls at 30 DEG C, and repeats to contaminate-be oxidized 6 times to silk fabric; After repeating to contaminate-be oxidized 6 times, silk fabric is soaped: preparation detergent 209 is 1g/l, and sodium carbonate is the liquid of soaping of 1g/l, is put into by silk fabric and soaps in liquid, and soap 10min at 95 DEG C.Wash away the dyestuff of the not upper dye in surface after soaping, improve the colour fastness of silk fabric.Dry after soaping, dry the natural indigo dyeing silk fabric of rear acquisition.
(2) natural indigo dyeing silk fabric extract is extracted: get the natural indigo dyeing silk fabric of 1g, add 15ml methanol solution, be immersed in completely in methanol solution by natural indigo dyeing silk fabric; Then at 50 DEG C, extract 20min, be extracted liquid, extract is placed in quartz colorimetric utensil;
(3) fluorometric investigation: get extract and be placed in fluorospectrophotometer, three-dimensional fluorescence method is adopted to carry out fluorometric investigation to extract, the test parameter of fluorospectrophotometer is first regulated to be: to excite slit width: 5nm, launch slit width: 4nm, photomultiplier tube signal: 350V, and determine that scanning wavelength is 200 ~ 780nm; Then scan extract, obtain the three-dimensional fluorescence spectrum figure as Fig. 1 in accompanying drawing,
As shown in Figure 1, there is the emission peak of feature in the extract of natural indigo dyeing silk fabric, and fluorescence intensity is more weak at 495nm place, be 0.175.This is because indigo red and indigo in transconfiguration, indigo red stability is better than indigo, in reduction-oxidation process, the structure of indigo red can not change, and indigo red has less fluorescence property, cause the extract of natural indigo dyeing silk fabric to present certain fluorescence property, namely occur the emission peak of feature at 495nm place.
Reference examples
(1) indigo dyeing: adopt indigo dyeing method in embodiment, will synthesizing indigo dyestuff contaminate in silk fabric, obtains synthesizing indigo dyeing silk fabric
(2) synthesizing indigo dyeing silk fabric extract is extracted: get 1g synthesizing indigo dyeing silk fabric, add 15ml methanol solution, the silk fabric that dyeed by synthesizing indigo is immersed in methanol solution completely; Then at 50 DEG C, extract 20min, be extracted liquid, extract is placed in quartz colorimetric utensil;
(3) fluorometric investigation: get extract and be placed in fluorospectrophotometer, three-dimensional fluorescence method is adopted to carry out fluorometric investigation to extract, the test parameter of fluorospectrophotometer is first regulated to be: to excite slit width: 5nm, launch slit width: 4nm, photomultiplier tube signal: 350V, and determine that scanning wavelength is 200 ~ 780nm; Then scan extract, obtain the three-dimensional fluorescence spectrum figure as Fig. 2 in accompanying drawing.
There is not the emission peak of feature in synthesizing indigo dyeing silk fabric extract as shown in Figure 2 within the scope of 200 ~ 780nm, this is mainly because synthesizing indigo comprises indigo and indigo white, indigo white do not have fluorescence property, in reduction-oxidation process indigo be reduced into indigo white, this causes the extract of synthesizing indigo dyeing silk fabric not present certain fluorescence property, does not namely have characteristic emission peak.It is wherein indigo that to be converted into indigo white principle as follows:
By comparative example and reference examples, indigo and indigo white do not have fluorescence property, indigo red has the fluorescence property of some strength, this causes the dye extract of silk fabric of the extract of natural indigo dyeing silk fabric and synthesizing indigo to occur certain fluorescent differences on three-dimensional fluorescence spectrum figure, can be used as the natural indigo discriminating foundation with synthesizing indigo.
These are only specific embodiments of the invention, but technical characteristic of the present invention is not limited thereto.Any based on the present invention, for solving substantially identical technical matters, realize substantially identical technique effect, done ground simple change, equivalent replacement or modification etc., be all covered by among protection scope of the present invention.
Claims (8)
1. a discrimination method for natural indigo dyeing silk fabric, first gets natural bipseudoindoxyl dye and silk fabric, it is characterized in that comprising following discrimination process:
(1) indigo dyeing: adopt reduction stain method, natural bipseudoindoxyl dye is dyeed to silk fabric, obtains natural indigo dyeing silk fabric;
(2) natural indigo dyeing silk fabric extract is extracted: get the natural indigo dyeing silk fabric of 1g, add 15ml methanol solution, be immersed in completely in methanol solution by natural indigo dyeing silk fabric; Then natural indigo dyeing silk fabric is extracted 15 ~ 20min at 50 DEG C, be extracted liquid, extract is placed in quartz colorimetric utensil;
(3) fluorometric investigation: get extract and be placed in fluorospectrophotometer, three-dimensional fluorescence method is adopted to carry out fluorometric investigation to extract, first regulate the test parameter of fluorospectrophotometer, comprise and excite slit width, transmitting slit width and photomultiplier tube signal, and determine that scanning wavelength is 200nm ~ 780nm; Then scan extract, obtain three-dimensional fluorescence spectrum figure.
2. the discrimination method of a kind of natural indigo dyeing silk fabric according to claim 1, it is characterized in that: in described step (1), the detailed process of indigo dyeing is: (a) reduces: first determine that bath raio is 1 ︰ 50, then accurately take natural bipseudoindoxyl dye 5% (o.w.f), Na
2s
2o
40.8g/l, NaOH0.6g/l, join natural bipseudoindoxyl dye in dye cup, and add water and mix well, and then in dye cup, adds Na
2s
2o
4, NaOH and water, stock vatting 30min obtains the green dye bath of transparent yellow; B () is oxidized: get 2.0g silk fabric and contaminate in dye bath completely, fully oxidized 2min after dip-dye 120s, and repeats to contaminate-be oxidized 6 times to silk fabric, finally soaps to silk fabric and dries, drying the natural indigo dyeing silk fabric of rear acquisition.
3. the discrimination method of a kind of natural indigo dyeing silk fabric according to claim 2, is characterized in that: add Na2S in reduction process in described step (a)
2o
4with the concrete grammar of NaOH be: first to contaminating in cup the Na adding 2/3
2s
2o
4, the NaOH of 2/3 and the water of 1/3, the initial temperature controlled in dye cup is 40 DEG C, is then warming up to 50 DEG C, stock vatting 10min at 50 DEG C; Then in dye cup, remaining 1/3NaOH, 1/3Na is added
2s
2o
4with 2/3 water, stock vatting 20min at 50 DEG C.
4. the discrimination method of a kind of natural indigo dyeing silk fabric according to claim 2, it is characterized in that: the detailed process of soaping in described step (b) oxidizing process is: preparation detergent 209 is 1g/l, sodium carbonate is the liquid of soaping of 1g/l, being put into by silk fabric soaps in liquid, and soap 10min at 95 DEG C.
5. the discrimination method of a kind of natural indigo dyeing silk fabric according to claim 1, is characterized in that: in described step (2), natural indigo dyeing silk fabric extracts 20min at 50 DEG C.
6. the discrimination method of a kind of natural indigo dyeing silk fabric according to claim 1, is characterized in that: excite slit width to be 5nm in described step (3).
7. the discrimination method of a kind of natural indigo dyeing silk fabric according to claim 1, is characterized in that: launching slit width in described step (3) is 5nm.
8. the discrimination method of a kind of natural indigo dyeing silk fabric according to claim 1, is characterized in that: in described step (3), photomultiplier tube signal is 350V.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106811995A (en) * | 2015-11-27 | 2017-06-09 | 苑少纯 | A kind of dyeing of indigo pigment dyeing silk fabric |
| CN109900647A (en) * | 2019-03-04 | 2019-06-18 | 青岛大学 | A kind of plant dyeing cotton fabric and chemical dyeing cotton fabric chromatography method for quick identification |
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| CN103459709A (en) * | 2011-03-31 | 2013-12-18 | 国际人造丝公司 | Disperse dyeing of textile fibers |
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2015
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| JP2000143992A (en) * | 1998-11-09 | 2000-05-26 | Free Zone:Kk | Silk of wild silkworm for cutting uv including natural dye and material utilizing the same and production of the same |
| CN103459709A (en) * | 2011-03-31 | 2013-12-18 | 国际人造丝公司 | Disperse dyeing of textile fibers |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106811995A (en) * | 2015-11-27 | 2017-06-09 | 苑少纯 | A kind of dyeing of indigo pigment dyeing silk fabric |
| 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 |
| CN109900647A (en) * | 2019-03-04 | 2019-06-18 | 青岛大学 | A kind of plant dyeing cotton fabric and chemical dyeing cotton fabric chromatography method for quick identification |
| 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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