CN112903667B - Method for rapidly identifying natural dye and synthetic dye - Google Patents

Method for rapidly identifying natural dye and synthetic dye Download PDF

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CN112903667B
CN112903667B CN202110068046.7A CN202110068046A CN112903667B CN 112903667 B CN112903667 B CN 112903667B CN 202110068046 A CN202110068046 A CN 202110068046A CN 112903667 B CN112903667 B CN 112903667B
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CN112903667A (en
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韩海涛
金子恒
文雁君
李轩
焦军伟
张二娟
宋超
尹慧云
华向美
董理
周迎春
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HENAN ZHONGDA BIOLOGICAL ENGINEERING CO LTD
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Abstract

The invention belongs to the field of chemical detection, and particularly relates to a method for rapidly identifying natural dye and synthetic dye. According to the method, ferric chloride solution and nitric acid solution are selected as identification reagents, different natural dyes and synthetic dyes are distinguished through three aspects of different reagents, different reaction time and color change after reaction, the method is simple and quick to operate, special equipment is not needed, the time consumption is short, the result can be obtained only by a single sample for 30min at most, and the method is not only suitable for rapid qualitative detection on a quality inspection spot, but also suitable for mass simultaneous detection, and can obviously improve the detection efficiency.

Description

Method for rapidly identifying natural dye and synthetic dye
Technical Field
The invention belongs to the field of chemical detection, and particularly relates to a method for rapidly identifying natural dye and synthetic dye.
Background
The natural pigment is a substance extracted from the root, stem, leaf, flower, fruit, seed, etc. of a plant or from an animal and used for dyeing, and is classified into 7 types of pigments, such as red, yellow, blue, green, purple, black and brown, according to the color system. Natural pigments are used in a wide variety of fields, especially in the food field. At present, most of dyes commonly used for dyeing in the textile printing and dyeing field are synthetic dyes. In fact, natural pigments have a long history of application as dyes in textile printing and dyeing fields, wherein the history of application of natural dyes in China has been thousands of years, and natural dyes have been the mainstream of ancient dyeing processes in China. In the 19 th century, with the development of textile industry, natural dyes cannot meet the rapidly growing dye demand, and compared with natural dyes, synthetic dyes have the advantages of colorful color, complete color spectrum, low cost, high color fastness, simple dyeing process and the like, and the increasingly-increased variety of synthetic dyes and the mature process of the process lead the dyeing industry and the textile industry to be improved dramatically, and the synthetic dyes gradually replace the main angle position of the natural dyes in the textile dyeing field.
With the improvement of social development and the living standard of people, people pursue natural and healthy living concepts, the meaning of textiles is expanded from body-shielding cold prevention to functions of attractive appearance, fashion, health, environmental protection and the like, the pollution problem of synthetic dyes to the environment is increasingly prominent, the potential injury to human bodies is also considered important, natural dyes are nontoxic and harmless, natural and elegant, antibacterial and maintenance and other excellent qualities are achieved, and the textile has the advantages of being attractive and popular in the textile printing and dyeing field, and is widely applied to the preparation of various textiles with high added value.
However, based on the high value of natural dyes in high-end markets, a large number of fake textiles which are called to be dyed by the natural dyes are emerging in the markets, so that not only are the rights and interests of consumers influenced, but also the interests of genuine manufacturers are greatly influenced, the normal market order is disturbed, and meanwhile, the popularization of the natural dye textiles is hindered, so that the identification of the textile dyes as the natural dyes or the synthetic dyes has important significance.
At present, the method for identifying the textile dye as the natural dye can be divided into a chemical reagent identification method and an instrument identification method according to the identification means, wherein the chemical reagent identification method achieves the purpose of preliminary identification according to the difference of color development reaction between the natural dye with different structures and properties and chemical reagents such as acid and alkali; the instrument identification method is to identify the dyes according to the difference of different natural dyes in the characteristic spectrogram, and mainly comprises a high performance liquid chromatography, a thin layer chromatography, a laser Raman spectroscopy, a micro optical fiber spectroscopy and the like. The latter, although more accurate, is costly and time consuming and not suitable for rapid detection in the field.
Disclosure of Invention
In order to overcome the defects and disadvantages of long time consumption, high cost, incapability of distinguishing multiple dyes simultaneously and the like in the existing technology for distinguishing the natural dye from the synthetic dye, the invention aims to provide a method for quickly distinguishing the natural dye from the synthetic dye.
The aim of the invention is achieved by the following technical scheme:
a method for rapidly identifying a natural dye and a synthetic dye, comprising the steps of:
(1) Taking a textile to be detected, selecting a certain area of the textile to be detected as a reaction area 1, and dropwise adding a reagent A on the reaction area 1 for reaction, wherein the reagent A is nitric acid solution, and observing the condition of color change and fading of the reaction area 1 in the reaction process;
(2) Selecting another area of the textile to be tested in the step (1) as a reaction area 2, and dropwise adding a reagent B on the reaction area 2 for reaction, wherein the reagent B is ferric chloride solution, and observing the condition of color change and fading of the reaction area 2 in the reaction process;
(3) Judging the dye type according to the color change conditions in the steps (1) and (2), wherein:
(1) after the reagent A and the reagent B are respectively dripped to react for at least 30min, the reaction zone 1 and the reaction zone 2 are not discolored and discolored, and the synthetic dye is obtained;
(2) when the reaction area 1 turns yellow after the reaction of the dropwise adding reagent A for 1-3 min, and the reaction area 2 turns brown after the reaction of the dropwise adding reagent B for 3-5 min, the madder dye is obtained;
(3) when the reaction area 1 does not have color change and fading after the reaction of the dropwise adding reagent A for at least 30min, and the reaction area 2 has browning after the reaction of the dropwise adding reagent B for 1-5 min, the color change is catechin dye or gallnut dye;
(4) when the reaction area 1 is discolored after the reaction of the dropwise adding of the reagent A for 1-5 min, and the reaction area 2 is browned after the reaction of the dropwise adding of the reagent B for 1-2 min, the color is myrobalan, pericarpium Granati, rubber shell, chestnut shell or cochineal dye;
(5) when the reaction area 1 is discolored after the reaction of the dropwise adding reagent A for 1-30 min, and meanwhile, when the reaction area 2 is not discolored and discolored after the reaction of the dropwise adding reagent B for at least 30min, the dye is gardenia yellow or gardenia blue dye;
(6) when the reaction area 1 turns red after the reaction of the dropwise adding reagent A for 1-10 min and the color is faded after the reaction of the dropwise adding reagent A for 15-30 min, and meanwhile, the reaction area 2 does not change color and fade after the reaction of the dropwise adding reagent B for at least 30min, the carmine dye is obtained;
(7) when the reaction area 1 is discolored after the reaction of the dropwise adding reagent A for 5-8 min, and the reaction area 2 is browned after the reaction of the dropwise adding reagent B for 5-10 min, the cocoa dye is obtained;
preferably, when the reaction area 1 is not discolored and discolored after the reaction of the dropwise adding reagent A for at least 30min, and the reaction area 2 is browned after the reaction of the dropwise adding reagent B for 4-5 min, the catechin is obtained; when the reaction area 1 is not discolored and discolored after the reaction of the dropwise adding reagent A for at least 30min, and the reaction area 2 is browned after the reaction of the dropwise adding reagent B for 1-2 min, the Chinese gall dye is obtained;
preferably, the gardenia yellow dye is obtained when the reaction area 1 is discolored after the reaction of dropwise adding the reagent A for 30min and the reaction area 2 is not discolored and discolored after the reaction of dropwise adding the reagent B for at least 30 min; when the reaction area 1 is discolored after the reaction of the dropwise adding reagent A for 1-3 min, and meanwhile, when the reaction area 2 is not discolored and discolored after the reaction of the dropwise adding reagent B for at least 30min, the gardenia blue dye is obtained;
the synthetic dye is cationic fluorescent yellow 4GL 500%, cationic blue X-GRRL, direct gray D, red base B, reactive brilliant yellow K-4GL, acid red P-5BL or acid yellow NM-5RL;
preferably, the fabric of the textile to be tested in the step (1) is cotton;
preferably, the concentration of the nitric acid solution in the step (1) is 1-20% (w/w);
preferably, the concentration of the nitric acid solution in step (1) is preferably 10% (w/w);
preferably, the concentration of the ferric chloride solution in the step (2) is preferably 0.1-10% (w/w);
preferably, the concentration of the ferric chloride solution in step (2) is preferably 5% (w/w);
compared with the prior art, the invention has the following advantages and effects:
(1) The method selects ferric chloride solution and nitric acid solution as identification reagents, and distinguishes different natural dyes and synthetic dyes through three aspects of different reagents, different reaction time and color change after reaction.
(2) The method selects the ferric chloride solution and the nitric acid solution as the identification reagent, is suitable for identifying different natural dyes and synthetic dyes of cotton textiles, is simple and quick in detection method operation, does not need special equipment, is short in time consumption, can obtain a result only by 30 minutes at most for a single sample, is suitable for quick qualitative detection on a quality inspection spot, is suitable for mass simultaneous detection, and can obviously improve detection efficiency.
(3) The method for rapidly identifying the natural dye and the synthetic dye provided by the invention only needs two common reagents of ferric chloride solution and nitric acid solution, has low cost and remarkable effect, and provides a simple and effective detection method for identifying the natural dye and the synthetic dye.
(4) The method for rapidly identifying the natural dye and the synthetic dye provided by the invention does not need to use high performance liquid chromatography, thin layer chromatography, laser Raman spectrum, micro optical fiber spectrum and other technologies and equipment, and the result only needs to be observed by naked eyes, does not need to carry out complex data processing and analysis, and is wider in applicable population and stronger in popularization.
(5) The method for rapidly identifying the natural dye and the synthetic dye provided by the invention has wider identification variety, and can identify and distinguish at least 12 natural dyes and 7 synthetic dyes.
Drawings
Fig. 1 is a graph showing the result of discoloration of cotton textiles dyed with madder by dropping nitric acid solutions and ferric chloride solutions of different concentrations.
Fig. 2 is a graph of the color fading and color changing results of cotton textiles dyed by myrobalan after adding nitric acid solutions and ferric chloride solutions with different concentrations.
Fig. 3 is a graph showing the result of discoloration of cotton textiles dyed with grenadine, after dropping nitric acid solutions and ferric chloride solutions of different concentrations.
Fig. 4 is a graph of the color fading and discoloration results of cotton textiles dyed with rubber shells after the nitric acid solution and ferric chloride solution with different concentrations are added dropwise.
Fig. 5 is a graph showing the result of discoloration after dropping nitric acid solutions and ferric chloride solutions with different concentrations into cotton textiles dyed with chestnut shells.
Fig. 6 is a graph of the color fading and discoloration results of cotton textiles dyed with gardenia yellow after dropping nitric acid solutions and ferric chloride solutions with different concentrations.
Fig. 7 is a graph of the color fading and discoloration results of cotton textiles dyed with gardenia blue after dropping nitric acid solutions and ferric chloride solutions with different concentrations.
FIG. 8 is a graph of the color change and fade results for cotton textiles dyed with cochineal by adding different concentrations of nitric acid solution and ferric chloride solution.
Fig. 9 is a graph of the color fading and color changing results of cotton textiles dyed with annatto after dropping nitric acid solutions and ferric chloride solutions of different concentrations.
Fig. 10 is a graph of the color fading and discoloration results after dropping nitric acid solutions and ferric chloride solutions of different concentrations into cotton textiles using cocoa dyes.
Fig. 11 is a graph of the color fading and discoloration results of cotton textiles dyed with catechu, after dropping nitric acid solutions and ferric chloride solutions of different concentrations.
Fig. 12 is a graph showing the result of discoloration of cotton textiles dyed with nutgall after dropping nitric acid solutions and ferric chloride solutions of different concentrations.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but embodiments of the present invention are not limited thereto.
The percentages referred to in the examples are all mass percentages.
Example 1
(1) Cutting the cotton textile dyed by madder into seven squares with the same size by taking the cotton textile dyed by madder as an experimental object, and selecting the central area of the cotton textile after cutting as a reaction area;
(2) At room temperature, dropwise adding 10% nitric acid solution, 5% nitric acid solution and 1% nitric acid solution into the reaction areas of three cut cotton textiles respectively for reaction for 30min, observing the color and fading conditions of the reaction areas in the reaction process, and setting three repetitions for each concentration;
(3) At room temperature, ferric chloride solution with the concentration of 10%, 5%, 1% and 0.1% is respectively dripped into the reaction areas of the remaining four cut cotton textiles for reaction for 30min, and the color and fading conditions of the reaction areas are observed in the reaction process, and three repetitions are arranged for each concentration.
After the nitric acid solutions with different concentrations are adopted for reaction for 1-3 min, the three sample reaction areas are all discolored, wherein the reaction area is changed from red to yellow after 10% nitric acid treatment, and the reaction area is changed from red to orange after 5% nitric acid solution treatment;
after 3-5 min of reaction by adopting ferric chloride solutions with different concentrations, browning occurs in all three sample reaction areas, wherein the browning is serious after 10% and 5% of ferric chloride solutions are treated (figure 1).
Example 2
The procedure of example 1 was followed using the myrobalan dyed cotton textile as the subject.
After nitric acid solutions with different concentrations are adopted for reaction for 3-5 min, obvious fading appears in the three sample reaction areas;
after 1-2 min of reaction with ferric chloride solutions with different concentrations, obvious browning occurs in all three sample reaction areas (figure 2).
Example 3
The procedure of example 1 was followed using cotton textile dyed with pomegranate rind as the subject.
After the nitric acid solutions with different concentrations are adopted to react for 1-3 min, the three sample reaction areas are all discolored, wherein the reaction areas are seriously discolored after 10% nitric acid treatment;
after 1-2 min of reaction with ferric chloride solutions with different concentrations, obvious browning occurs in all three sample reaction areas (figure 3).
Example 4
The procedure of example 1 was followed using rubber-shell dyed cotton textiles as the subject.
After nitric acid solutions with different concentrations are adopted for reaction for 3-5 min, obvious fading appears in the three sample reaction areas;
after 1-2 min of reaction with ferric chloride solutions with different concentrations, obvious browning occurs in all three sample reaction areas (figure 4).
Example 5
The cotton textile dyed with chestnut shells is used as an experimental object, and other steps are the same as in example 1.
After nitric acid solutions with different concentrations are adopted for reaction for 1-3 min, obvious fading appears in the three sample reaction areas;
after 1-2 min of reaction with ferric chloride solutions with different concentrations, obvious browning occurs in all three sample reaction areas (figure 5).
Example 6
The cotton textile dyed with gardenia yellow was used as the subject, and the other steps were the same as in example 1.
After the nitric acid solutions with different concentrations are adopted for 30min, only the reaction area is obviously discolored to be white after the treatment of the 10% nitric acid solution, and the reaction area is unchanged after the treatment of the 5% nitric acid solution and the 1% nitric acid solution;
after 30min of reaction with ferric chloride solutions of different concentrations, no obvious discoloration and fading occurred in the reaction areas of the three samples (fig. 6).
Example 7
The procedure of example 1 was followed using gardenia blue dyed cotton textiles as the subject.
After nitric acid solutions with different concentrations are adopted for reaction for 1-3 min, only the reaction area is obviously discolored to be white after being treated by 10% nitric acid solution, and the reaction area is not obviously changed after being treated by 5% nitric acid solution and 1% nitric acid solution;
after 30min of reaction with ferric chloride solutions of different concentrations, no obvious discoloration and fading occurred in the reaction areas of the three samples (fig. 7).
Example 8
Cochineal dyed cotton textiles were used as subjects, with the other steps being as in example 1.
After nitric acid solutions with different concentrations are adopted for reaction for 1-3 min, the three sample reaction areas are all discolored, and the reaction areas are obviously discolored to be white after being treated by 10% nitric acid solution;
after 1-2 min of reaction with ferric chloride solutions with different concentrations, obvious browning occurs in all three sample reaction areas (figure 8).
Example 9
Using annatto-dyed cotton textiles as the subject, the other procedure was as in example 1.
After the nitric acid solutions with different concentrations are adopted for reaction for 1 to 10 minutes, the reaction areas of three samples are changed into red, and obvious fading is gradually formed after 15 to 30 minutes;
after 30min of reaction with ferric chloride solutions of different concentrations, no obvious discoloration and fading occurred in the reaction areas of the three samples (fig. 9).
Example 10
The procedure of example 1 was followed using a cocoa-dyed cotton textile as the subject.
After nitric acid solutions with different concentrations are adopted for reaction for 5-8 min, the three sample reaction areas are all discolored;
after 5-10 min of reaction with ferric chloride solutions with different concentrations, browning occurs in all three sample reaction areas (figure 10).
Example 11
The procedure of example 1 was followed using a cotton textile dyed with catechu as the subject.
After nitric acid solutions with different concentrations are adopted for reaction for 30min, the three sample reaction areas are not subjected to color change and fading;
after 4-5 min of reaction with ferric chloride solutions with different concentrations, obvious browning occurs in all three sample reaction areas (figure 11).
Example 12
The procedure of example 1 was followed using the cotton textile dyed with nutgall as the subject.
After nitric acid solutions with different concentrations are adopted for reaction for 30min, obvious color and fading do not occur in the reaction areas of the three samples;
after 1-2 min of reaction with ferric chloride solutions with different concentrations, obvious browning occurs in all three sample reaction areas (figure 12).
Example 13
The procedure of example 1 was followed except that cotton textiles of cationic fluorescent yellow 4GL 500%, cationic blue X-GRRL, direct gray D, red base B, reactive yellow K-4GL, acid red P-5BL, and acid yellow NM-5RL were used as subjects.
After nitric acid solutions with different concentrations are adopted for reaction for 30min, no obvious color change and fading occur in all sample reaction areas;
after the ferric chloride solutions with different concentrations are adopted for reaction for 30min, no obvious discoloration and fading occur in all sample reaction areas.
Table 1 optimal identification reagent and identification result thereof
Figure BDA0002904920830000081
TABLE 2 identification of synthetic dyes
Figure BDA0002904920830000082
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Figure BDA0002904920830000091
As can be seen from tables 1 and 2, the dyeing of cotton textiles with synthetic dyes treated with ferric chloride solution and nitric acid solution as identification agents did not undergo discoloration and fading; and cotton textiles dyed by different natural dyes are treated by adopting ferric chloride solution and nitric acid solution as identification reagents, so that different color-changing and fading conditions can occur, and the color-changing and fading time can be different according to the different dyes.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.

Claims (5)

1. A method for rapidly identifying natural dyes and synthetic dyes, comprising the steps of:
(1) Taking a textile to be detected, selecting a certain area of the textile to be detected as a reaction area 1, and dropwise adding a reagent A on the reaction area 1 for reaction, wherein the reagent A is nitric acid solution, and observing the condition of color change and fading of the reaction area 1 in the reaction process;
(2) Selecting another area of the textile to be tested in the step (1) as a reaction area 2, and dropwise adding a reagent B on the reaction area 2 for reaction, wherein the reagent B is ferric chloride solution, and observing the condition of color change and fading of the reaction area 2 in the reaction process;
(3) Judging the dye type according to the color change conditions in the steps (1) and (2), wherein:
(1) after the reagent A and the reagent B are respectively dripped to react for at least 30min, the reaction zone 1 and the reaction zone 2 are not discolored and discolored, and the synthetic dye is obtained;
(2) when the reaction area 1 turns yellow after the reaction of the dropwise adding reagent A for 1-3 min, and the reaction area 2 turns brown after the reaction of the dropwise adding reagent B for 3-5 min, the madder dye is obtained;
(3) when the reaction area 1 does not have color change and fading after the reaction of the dropwise adding reagent A for at least 30min, and the reaction area 2 has browning after the reaction of the dropwise adding reagent B for 1-5 min, the color change is catechin or gallnut;
(4) when the reaction area 1 is discolored after the reaction of the dropwise adding of the reagent A for 1-5 min, and the reaction area 2 is browned after the reaction of the dropwise adding of the reagent B for 1-2 min, the color is myrobalan, pericarpium Granati, rubber shell, chestnut shell or cochineal dye;
(5) when the reaction area 1 is discolored after the reaction of the dropwise adding reagent A for 1-30 min, and meanwhile, when the reaction area 2 is not discolored and discolored after the reaction of the dropwise adding reagent B for at least 30min, the dye is gardenia yellow or gardenia blue dye;
(6) when the reaction area 1 turns red after the reaction of the dropwise adding reagent A for 1-10 min and the reaction area turns red after the reaction for 15-30 min, and meanwhile, when the reaction area 2 does not turn color and fade after the reaction of the dropwise adding reagent B for at least 30min, the carmine dye is obtained;
(7) fading occurs in the reaction area 1 after the reaction of dropwise adding the reagent A for 5-8 min, and meanwhile, browning occurs in the reaction area 2 after the reaction of dropwise adding the reagent B for 5-10 min, so that the cocoa dye is obtained;
the concentration of the nitric acid solution in the step (1) is 10% w/w;
the concentration of the ferric chloride solution in the step (2) is 5% w/w.
2. The method for rapid identification of natural and synthetic dyes according to claim 1, wherein:
when the reaction area 1 does not fade or change color after the reaction of the dropwise adding reagent A for at least 30min, and the reaction area 2 is brown after the reaction of the dropwise adding reagent B for 4-5 min, the catechin is obtained; and when the reaction area 1 is not discolored and discolored after the reaction of the dropwise adding reagent A for at least 30min, and the reaction area 2 is browned after the reaction of the dropwise adding reagent B for 1-2 min, the Chinese gall dye is obtained.
3. The method for rapid identification of natural and synthetic dyes according to claim 1, wherein:
when the reaction area 1 is discolored after the reaction of the dropwise adding reagent A for 30min, and meanwhile, the reaction area 2 is not discolored and discolored after the reaction of the dropwise adding reagent B for at least 30min, the gardenia yellow dye is obtained; and (3) when the reagent A is added dropwise for 1-3 min, the reaction area 1 is discolored, and meanwhile, when the reagent B is added dropwise for at least 30min, the reaction area 2 is not discolored and discolored, so that the gardenia blue dye is obtained.
4. The method for rapid identification of natural and synthetic dyes according to claim 1, wherein:
the synthetic dye is cationic fluorescent yellow 4GL 500%, cationic blue X-GRRL, direct gray D, red base B, reactive brilliant yellow K-4GL, acid red P-5BL and acid yellow NM-5RL.
5. The method for rapid identification of natural and synthetic dyes according to claim 1, wherein:
the fabric of the textile to be tested in the step (1) is cotton.
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