CN105136772A - Raman spectrum discriminating method of natural dyeing silk fabrics - Google Patents
Raman spectrum discriminating method of natural dyeing silk fabrics Download PDFInfo
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Abstract
The invention discloses a Raman spectrum discriminating method of natural dyeing silk fabrics, and comprises the following steps: (1) indigo dyeing: a natural indigo dye is adopted to dye silk fabrics with a reduction dyeing method, and a sample 1, a sample 2, and a sample 3 are obtained; (2) a copper coin substrate is prepared; (3) UV aging: the sample 2 and sample 3 are placed in a UV aging test machine for aging for a period of time; and (4) Raman spectrum test: the substrate is placed on a Fourier infrared Raman spectrometer, then the sample 1, sample 2, sample 3 are placed in batches in the Fourier infrared Raman spectrometer to acquire Raman spectrums. In the invention, non-invasive Raman spectrum technology is adopted for performing characterization test for natural indigo dyed silk fabrics and synthetic indigo dyed silk fabrics, and achieves the goal for quickly discriminating the fabrics, and has a significance in food development, fabric dyeing and discrimination and maintenance for ancient textiles.
Description
Technical field
The present invention relates to chemical dye and differentiate field, especially relate to the Raman spectrum 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 synthetic dyestuffs.Compared with other natural dyes, natural indigo middle pigment composition is few, only main containing indigo and indigo red two kinds of pigmentary structures (indigo as follows with indigo red molecular formula):
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 comprises following two kinds: first, thin-layer chromatography, oxidizing process is adopted to carry out discriminating research to natural indigo dyeing bafta and synthesizing indigo dyed cotton fabric, the method belongs to and damages test, produce certain damage, and the degree of discrimination is not high to fabric.The second, only adopt near-infrared spectrum technique to carrying out discriminating research to natural indigo dyeing bafta and synthesizing indigo dyed cotton fabric, there is the problem that discrimination method is single.
Summary of the invention
The object of the present invention is to provide the Raman spectrum discrimination method of natural indigo dyeing silk fabric, adopt harmless Raman spectroscopy to carry out characterization test to natural indigo dyeing silk fabric and synthesizing indigo dyeing silk fabric.Dye difference that silk fabric shows in Raman spectrum as differentiating foundation according to natural indigo dyeing silk fabric and synthesizing indigo.Thus reach the object differentiated fast, in the discriminating of food development, textile dyeing and ancient textiles and significant in safeguarding.
In order to solve upper technical matters, adopt following technical scheme:
The Raman spectrum discrimination method of natural indigo dyeing silk fabric, is characterized in that comprising the steps:
(1) indigo dyeing: adopt reduction stain method, natural bipseudoindoxyl dye is dyeed to silk fabric, obtained natural indigo dyeing silk fabric, and the natural indigo dyeing silk fabric of cutting, obtain sample 1, sample 2 and sample 3;
(2) prepare substrate: first get copper coin, rear polishing is cleaned to the surface of copper coin, then assembles electrolytic cell, copper coin is joined in electrolytic cell, oxidation-reduction 50-60min in electrolytic cell, take out copper coin, copper coin rough surface; Then dust-proof exposure 3-5h under copper coin being placed in room temperature, allows copper coin autoxidation;
(3) ultraviolet light and aging:
A, be first placed in ultraviolet light accelerated weathering accelerator by sample 2, the temperature controlling ultraviolet light accelerated weathering accelerator is 50-55 DEG C, and ultraviolet light irradiation intensity is 0.85-0.92Wm
-2, continuous illumination 24h, then takes out sample 2 for subsequent use;
B, be first placed in ultraviolet light accelerated weathering accelerator by sample 3, the temperature controlling ultraviolet light accelerated weathering accelerator is 60-65 DEG C, and ultraviolet light irradiation intensity is 0.85-0.92Wm
-2, continuous illumination 48h, then takes out sample 3 for subsequent use;
(4) Raman spectrum test: first substrate is mounted on fourier-transform infrared-Raman spectrometer, then sample 1, sample 2 and sample 3 are joined fourier-transform infrared-Raman spectrometer in batches, obtained the Raman spectrogram of the Raman spectrogram of sample 1, the Raman spectrogram of sample 2 and sample 3 by test.
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
41.2g/l, Na
2cO
20.6g/l, joins natural bipseudoindoxyl dye in dye cup, and adds water and mix well, and then in dye cup, adds Na
2s
2o
4, Na
2cO
2and water, stock vatting 35-40min 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 60s completely, and repeat to contaminate-be oxidized 8 times to silk fabric, finally silk fabric soaped and dry, drying the natural indigo dyeing silk fabric of rear acquisition.Oxide-reduction method dyes, and dyeing is fast, and dye-uptake is high, even dyeing, is particularly suitable for the silk fabric that dyes.
Preferably, in step (a), in reduction process, add Na
2s
2o
4with Na
2cO
2concrete grammar be: in dye cup, first add the Na of 2/3
2s
2o
4, 2/3 Na
2cO
2with the water of 1/3, the initial temperature in dye cup is 20 DEG C, and be then warming up to 50 DEG C gradually, heating rate is 5 DEG C/min, stock vatting 10min at 50 DEG C; Then in dye cup, remaining 1/3Na is added
2cO
2, 1/3Na
2s
2o
4with 2/3 water, stock vatting 25-30min at 50 DEG C.In reducing dye process, add Na in batches
2s
2o
4, Na
2cO
2and water, be conducive to above-mentioned auxiliary agent and better mix with dyestuff, improve dye-uptake.
Preferably, the detailed process of soaping in step (b) oxidizing process is: preparation detergent 209 is 1.5g/l, Na
2cO
2for the liquid of soaping of 1g/l, put into by silk fabric and soap in liquid, soap 10min at 95 DEG C.The dyestuff of the not upper dye in silk fabric surface can be washed away, improve colour fastness and the level-dyeing property of silk fabric.
Preferably, in the electrolytic cell of step (2), electrolyte is potassium chloride or sulfuric acid.Potassium chloride and sulfuric acid are not only drawn materials conveniently, with low cost, and electrolysis effectiveness is desirable, significantly can accelerate electrolytic process.
Preferably, in step (4), when fourier-transform infrared-Raman spectrometer scanning samples 1, sample 2 and sample 3, sweep signal all cumulative 32 times.Degree of accuracy and the accuracy of Raman spectrum test can be significantly improved by cumulative scan signal.
Preferably, in step (4), the spectral resolution of fourier-transform infrared-Raman spectrometer is set to 4cm
-1.In this spectral resolution, the Raman spectrogram of sample 1, sample 2 and sample 3 is the most clear
Preferably, in step (4), the laser power of fourier-transform infrared-Raman spectrometer is set to 100-200mW.Within the scope of this laser power, fourier-transform infrared-Raman spectrometer tests the best results of natural indigo dyeing silk fabric and synthesizing indigo dyeing silk fabric.
Owing to adopting technique scheme, there is following beneficial effect:
The present invention is the Raman spectrum discrimination method of natural indigo dyeing silk fabric, adopts harmless Raman spectroscopy to carry out characterization test to natural indigo dyeing silk fabric and synthesizing indigo dyeing silk fabric.Dye difference that silk fabric shows in Raman spectrum as differentiating foundation according to natural indigo dyeing silk fabric and synthesizing indigo.Thus reach the object differentiated fast, in the discriminating of food development, textile dyeing and ancient textiles and significant in safeguarding.Its beneficial effect be embodied in following some:
1, the discrimination method that the present invention adopts is Undamaged determination, significantly reduces raw-material loss in differentiating, avoids waste, reduce and differentiate cost.
2, compared with testing with existing Raman spectrum, invention increases copper substrate in fourier-transform infrared-Raman spectrometer, significantly strengthen incident excitation light intensity in Raman spectrum test, improve degree of accuracy and the accuracy of Raman spectrum test.
3, sample 2 and sample 3 are placed in burin-in process in ultraviolet light accelerated weathering accelerator, can analogy to using the silk fabric after the long period, make usable range of the present invention wider, not only can differentiate the natural indigo dyeing silk fabric of just dyeing, also the natural indigo dyeing silk fabric after using longer a period of time can be differentiated, its difference is only embodied in characteristic peak signal intensity, the signal strength weakening of aging rear characteristic peak.
4, Raman spectra test method is easy and simple to handle, differentiates that speed is fast, practical, is suitable for developing.
Accompanying drawing illustrates:
Fig. 1 is the Raman spectrogram of sample 1 and sample 4 in the present invention;
Fig. 2 is the Raman spectrogram of sample 2 and sample 5 in the present invention;
Fig. 3 is the Raman spectrogram of sample 3 and sample 6 in the present invention.
The wherein natural indigo dyeing silk fabric of natural indigo expression in Fig. 1, Fig. 2, Fig. 3, synthesizing indigo represents synthesizing indigo dyeing silk fabric.
Embodiment
The present invention adopts harmless Raman spectroscopy to carry out characterization test to natural indigo dyeing silk fabric and synthesizing indigo dyeing silk fabric.Dye difference that silk fabric shows in Raman spectrum as differentiating foundation according to natural indigo dyeing silk fabric and synthesizing indigo, thus reaches the object differentiated fast.
The present invention needs to prepare following experiment material, medicine and instrument:
Material: copper coin, silk fabric (50g/m
2), natural bipseudoindoxyl dye and synthesizing indigo dyestuff;
Medicine: potassium chloride, sulfuric acid, Na
2s
2o
4, Na
2cO
2and detergent 209;
Instrument: fourier-transform infrared-Raman spectrometer and ultraviolet light accelerated weathering accelerator.
Below in conjunction with specific embodiment, the invention will be further described:
Embodiment:
(1) indigo dyeing: adopt reduction stain method, natural bipseudoindoxyl dye is dyeed to silk fabric, dyeing and formula are as following table:
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
41.2g/l, Na
2cO
20.6g/l, joins natural bipseudoindoxyl dye in dye cup, and adds water and mix well; Then in dye cup, first add the Na of 2/3
2s
2o
4, 2/3 Na
2cO
2with the water of 1/3, the initial temperature in dye cup is 20 DEG C, and be then warming up to 50 DEG C gradually, heating rate is 5 DEG C/min, stock vatting 10min at 50 DEG C; Then in dye cup, remaining 1/3Na is added
2cO
2, 1/3Na
2s
2o
4with the water of 2/3, stock vatting 30min 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 60s completely, during dip-dye, temperature controls at 30 DEG C, and repeats to contaminate-be oxidized 8 times to silk fabric, then silk fabric is soaped: preparation detergent 209 is 1.5g/l, Na
2cO
2for the liquid of soaping of 1g/l, put into by silk fabric and soap in liquid, soap 10min at 95 DEG C, can wash away the dyestuff of the not upper dye in silk fabric surface.Dry after soaping, dry the natural indigo dyeing silk fabric of rear acquisition.Oxide-reduction method dyes, and dyeing is fast, and dye-uptake is high, even dyeing, is particularly suitable for the silk fabric that dyes.
(c) cutting natural indigo dyeing silk fabric: the center section getting natural indigo dyeing silk fabric during cutting, is cut into the oblong-shaped of 20*10, thus obtain sample 1, sample 2 and sample 3.
(2) prepare substrate: first get copper coin, rear polishing is cleaned to the surface of copper coin, then assembles electrolytic cell, in electrolytic cell, add sulfuric acid as electrolyte.Copper coin is joined electrolytic cell, is immersed in electrolyte, copper coin is oxidation-reduction 60min in electrolytic cell, and in oxidation-reduction process, the copper on copper coin surface loses electronics, with Cu
2+form be present in electrolytic cell; Final taking-up copper coin, copper coin is after oxidation-reduction process, and copper coin surface becomes coarse; Then dust-proof exposure 5h under copper coin being placed in room temperature, allows copper coin autoxidation, after autoxidation, copper coin is stayed do for subsequent use;
(3) ultraviolet light and aging:
A, be first placed in ultraviolet light accelerated weathering accelerator by sample 2, the temperature controlling ultraviolet light accelerated weathering accelerator is 50 DEG C, and ultraviolet light irradiation intensity is 0.9Wm
-2, continuous illumination 24h, then takes out sample 2 for subsequent use;
B, be first placed in ultraviolet light accelerated weathering accelerator by sample 3, the temperature controlling ultraviolet light accelerated weathering accelerator is 60 DEG C, and ultraviolet light irradiation intensity is 0.9Wm
-2, continuous illumination 48h, then takes out sample 3 for subsequent use;
(4) Raman spectrum test: first substrate is mounted on fourier-transform infrared-Raman spectrometer, the spectral resolution of fourier-transform infrared-Raman spectrometer is set to 4cm
-1, the laser power of fourier-transform infrared-Raman spectrometer is set to 100-200mW.Then sample 1, sample 2 and sample 3 are joined fourier-transform infrared-Raman spectrometer in batches, when scanning samples 1, sample 2 and sample 3, sweep signal all cumulative 32 times.The Raman spectrogram of the Raman spectrogram of final acquisition sample 1, the Raman spectrogram of sample 2 and sample 3.
From Fig. 1, Fig. 2 and Fig. 3 of Figure of description, the Raman spectrogram of sample 1, sample 2 and sample 3 is at 189cm
-1and 1573cm
-1there are two characteristic peaks at place.Because in natural bipseudoindoxyl dye, include indigo pigment and indigo red pigment.Both molecular formula is the same, is C
16h
10n
2o
2, but configuration isomers each other.The difference of isomers molecule can be detected, therefore at 189cm in Raman spectrogram
-1and 1573cm
-1there are two characteristic peaks at place.Meanwhile, after adding copper coin substrate, the signal of characteristic peak obviously strengthens.
Reference examples:
(1) adopt indigo dyeing method in embodiment, and replace natural bipseudoindoxyl dye with synthesizing indigo dyestuff, contaminate on synthesizing indigo dyestuff in silk fabric, thus obtain synthesizing indigo dyeing silk fabric.According to the method for cutting out cutting synthesizing indigo dyeing silk fabric of embodiment, thus obtain sample 4, sample 5 and sample 6.
(2) the copper coin substrate that embodiment is obtained can directly be adopted.
(3) ultraviolet light and aging:
A, be first placed in ultraviolet light accelerated weathering accelerator by sample 5, the temperature controlling ultraviolet light accelerated weathering accelerator is 50 DEG C, and ultraviolet light irradiation intensity is 0.9Wm
-2, continuous illumination 24h, then takes out sample 5 for subsequent use;
B, be first placed in ultraviolet light accelerated weathering accelerator by sample 6, the temperature controlling ultraviolet light accelerated weathering accelerator is 60 DEG C, and ultraviolet light irradiation intensity is 0.9Wm
-2, continuous illumination 48h, then takes out sample 6 for subsequent use;
(4) Raman spectrum test: first substrate is mounted on fourier-transform infrared-Raman spectrometer, the spectral resolution of fourier-transform infrared-Raman spectrometer is set to 4cm
-1, the laser power of fourier-transform infrared-Raman spectrometer is set to 100-200mW.Then sample 4, sample 5 and sample 6 are joined fourier-transform infrared-Raman spectrometer in batches, when scanning samples 4, sample 5 and sample 6, sweep signal all cumulative 32 times.The Raman spectrogram of the Raman spectrogram of final acquisition sample 4, the Raman spectrogram of sample 5 and sample 6.
From Fig. 1, Fig. 2 and Fig. 3 of Figure of description, the Raman spectrogram of sample 4, sample 5 and sample 6 is only at 1573cm
-1there is characteristic peak at place.Because in synthesizing indigo dyestuff, only include indigo pigment, be merely able at 1573cm in Raman spectrogram
-1place obtains characteristic peak.Meanwhile, after adding copper coin substrate, the signal of characteristic peak obviously strengthens.
Comparative example and reference examples known: can by 189cm
-1place's characteristic peak is as the foundation distinguishing natural indigo dyeing silk fabric and synthesizing indigo dyeing silk fabric.And after burin-in process, natural indigo dyeing silk fabric and synthesizing indigo dyeing silk fabric can be differentiated equally, the indigo red in natural bipseudoindoxyl dye can't be destroyed, but the signal intensity of its characteristic peak can weaken after weathering.
In addition natural indigo dyeing silk fabric and synthesizing indigo dye silk fabric except going out peak position to some extent except difference, and also different in peak shape, from Fig. 1, Fig. 2 and Fig. 3, natural indigo dyeing silk fabric is at 3300cm
-1-1400cm
-1in region, peak shape compares burr, have multiple irregular go out peak-to-peak signal, and synthesizing indigo dyeing silk fabric basic no signal in this region.This mainly because comparison of ingredients is many in natural bipseudoindoxyl dye, and only has a kind of indigo pigment, so the smoothness presented on Raman collection of illustrative plates is different in synthesizing indigo.By the situation of the Raman signal in these two regions, also can be used as the auxiliary discriminating foundation judging natural indigo dyeing silk fabric and synthesizing indigo dyeing silk fabric.
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. the Raman spectrum discrimination method of natural indigo dyeing silk fabric, is characterized in that comprising the steps:
(1) indigo dyeing: adopt reduction stain method, natural bipseudoindoxyl dye is dyeed to silk fabric, obtained natural indigo dyeing silk fabric, and the natural indigo dyeing silk fabric of cutting, obtain sample 1, sample 2 and sample 3;
(2) prepare substrate: first get copper coin, rear polishing is cleaned to the surface of copper coin, then assembles electrolytic cell, copper coin is joined in electrolytic cell, oxidation-reduction 50-60min in electrolytic cell, take out copper coin, copper coin rough surface; Then dust-proof exposure 3-5h under copper coin being placed in room temperature, allows copper coin autoxidation;
(3) ultraviolet light and aging:
A, be first placed in ultraviolet light accelerated weathering accelerator by sample 2, the temperature controlling ultraviolet light accelerated weathering accelerator is 50-55 DEG C, and ultraviolet light irradiation intensity is 0.85-0.92Wm
-2, continuous illumination 24h, then takes out sample 2 for subsequent use;
B, be first placed in ultraviolet light accelerated weathering accelerator by sample 3, the temperature controlling ultraviolet light accelerated weathering accelerator is 60-65 DEG C, and ultraviolet light irradiation intensity is 0.85-0.92Wm
-2, continuous illumination 48h, then takes out sample 3 for subsequent use;
(4) Raman spectrum test: first substrate is mounted on fourier-transform infrared-Raman spectrometer, then sample 1, sample 2 and sample 3 are joined fourier-transform infrared-Raman spectrometer in batches, obtained the Raman spectrogram of the Raman spectrogram of sample 1, the Raman spectrogram of sample 2 and sample 3 by test.
2. the Raman spectrum discrimination method 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
41.2g/l, Na
2cO
20.6g/l, joins natural bipseudoindoxyl dye in dye cup, and adds water and mix well, and then in dye cup, adds Na
2s
2o
4, Na
2cO
2and water, stock vatting 35-40min 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 60s completely, and repeat to contaminate-be oxidized 8 times to silk fabric, finally silk fabric soaped and dry, drying the natural indigo dyeing silk fabric of rear acquisition.
3. the Raman spectrum discrimination method of natural indigo dyeing silk fabric according to claim 2, is characterized in that: add Na in reduction process in described step (a)
2s
2o
4with Na
2cO
2concrete grammar be: in dye cup, first add the Na of 2/3
2s
2o
4, 2/3 Na
2cO
2with the water of 1/3, the initial temperature in dye cup is 20 DEG C, and be then warming up to 50 DEG C gradually, heating rate is 5 DEG C/min, stock vatting 10min at 50 DEG C; Then in dye cup, remaining 1/3Na is added
2cO
2, 1/3Na
2s
2o
4with 2/3 water, stock vatting 25-30min at 50 DEG C.
4. the Raman spectrum discrimination method of natural indigo dyeing silk fabric according to claim 2, is characterized in that: the detailed process of soaping in described step (b) oxidizing process is: preparation detergent 209 is 1.5g/l, Na
2cO
2for the liquid of soaping of 1g/l, put into by silk fabric and soap in liquid, soap 10min at 95 DEG C.
5. the Raman spectrum discrimination method of natural indigo dyeing silk fabric according to claim 1, is characterized in that: in the electrolytic cell of described step (2), electrolyte is potassium chloride or sulfuric acid.
6. the Raman spectrum discrimination method of natural indigo dyeing silk fabric according to claim 1, it is characterized in that: in described step (4), when fourier-transform infrared-Raman spectrometer scanning samples 1, sample 2 and sample 3, sweep signal all cumulative 32 times.
7. the Raman spectrum discrimination method of natural indigo dyeing silk fabric according to claim 1, is characterized in that: in described step (4), the spectral resolution of fourier-transform infrared-Raman spectrometer is set to 4cm
-1.
8. the Raman spectrum discrimination method of natural indigo dyeing silk fabric according to claim 1, is characterized in that: in described step (4), the laser power of fourier-transform infrared-Raman spectrometer is set to 100-200mW.
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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 |
| CN106770260A (en) * | 2017-01-22 | 2017-05-31 | 宁波市纤维检验所 | A kind of chemical method for differentiating bafta vegetable colour |
| CN108760712A (en) * | 2017-11-10 | 2018-11-06 | 天津大学 | Historical relic light injury determination method based on Raman spectrum analysis |
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| CN101629907A (en) * | 2009-08-03 | 2010-01-20 | 首都师范大学 | Method for authenticating inkpad of Chinese painting and calligraphy |
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| 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 |
| CN106770260A (en) * | 2017-01-22 | 2017-05-31 | 宁波市纤维检验所 | A kind of chemical method for differentiating bafta vegetable colour |
| CN106770260B (en) * | 2017-01-22 | 2019-05-03 | 宁波市纤维检验所 | A kind of chemical method identifying cotton fabric vegetable colour |
| CN108760712A (en) * | 2017-11-10 | 2018-11-06 | 天津大学 | Historical relic light injury determination method based on Raman spectrum analysis |
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| CN105136772B (en) | 2018-06-22 |
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