CN113529435A - Preparation method of purple dragon silk based on special dye - Google Patents
Preparation method of purple dragon silk based on special dye Download PDFInfo
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- CN113529435A CN113529435A CN202110150568.1A CN202110150568A CN113529435A CN 113529435 A CN113529435 A CN 113529435A CN 202110150568 A CN202110150568 A CN 202110150568A CN 113529435 A CN113529435 A CN 113529435A
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- purple
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- dragon silk
- silk
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/0056—Dyeing with polymeric dyes involving building the polymeric dyes on the fibres
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/28—Preparatory processes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B57/00—Other synthetic dyes of known constitution
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B69/00—Dyes not provided for by a single group of this subclass
- C09B69/10—Polymeric dyes; Reaction products of dyes with monomers or with macromolecular compounds
- C09B69/109—Polymeric dyes; Reaction products of dyes with monomers or with macromolecular compounds containing other specific dyes
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/008—Preparing dyes in situ
Abstract
The invention relates to a preparation method of purple dragon silk based on special dye, which comprises the steps of mixing o-phenylenediamine and tartaric acid in an ethanol solution, carrying out ultrasonic stirring, mixing and stirring with the dragon silk to prepare a four-component mixed solution, reacting at 175-185 ℃, cooling to room temperature, removing liquid by using an organic filter membrane, leaving the dyed dragon silk, cleaning residual solution, and drying to obtain the purple dragon silk. By adopting the invention, the covalent bond is formed by one-pot solvothermal reaction self-assembly, and the prepared nylon yarn has uniform color, stable structure and good biocompatibility, can be applied to the fields of information encryption, green dyeing and finishing and the like, and widens the application range of dyeing materials.
Description
Technical Field
The invention relates to a preparation method of purple Spiraria natans based on a special dye, and belongs to the field of special dye dyeing and finishing biomass fibers.
Background
The dragon silk is a popular environment-friendly material in recent years. The natural fiber of the dragon yarn is prepared by wet spinning. Because of good hygroscopicity, comfortable wearing and excellent spinnability, the dragon silk is often blended and interwoven with cotton, wool or various synthetic fibers, is used for various clothes and decorative textiles, and has good biodegradability, compatibility and renewability. The dragon silk plays an important role in life and production, and is mainly used for various textiles, clothes, blanket decorations and the like.
The dyeing dye for the dragon silk at present comprises reactive dye, direct dye, vat dye and the like, wherein the reactive dye is taken as the main material. A large amount of hydrolytic dye can be generated in the water-phase dyeing process of the conventional reactive dye, and a large amount of inorganic salt is required to be added in the dyeing process for accelerating the dyeing, so that the salt content of the dyed sewage is large, and the treatment difficulty of the printing and dyeing wastewater is greatly increased.
And different colors are traditionally needed to be modulated by color paste, and the traditional reactive dye ink is used for modulation, so that the reactive dye is easy to hydrolyze in the steaming process, and a large amount of hydrolytic dye is contained in the washing wastewater, so that the environment is polluted.
Compared with the traditional organic dye, the special dye has unique biological characteristics, the strength and stability of the special dye are higher than those of the dye, and the photobleaching phenomenon is less than that of the dye; meanwhile, the modified special dye also has certain biocompatibility, can be subjected to specific connection, and can be used for biological living body marking and detection. The probe as a novel special dye plays an important role in the research fields of biomolecule detection, multicolor marking, dyeing and finishing of the dragon silk and the like.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a preparation method of purple dragon silk based on special dye, the dragon silk obtained by adopting chemical reaction has the characteristics of bright color, original shape maintenance, simple preparation process and low toxicity.
The technical scheme adopted by the invention is as follows: a preparation method of purple Spiraria natans based on special dyes is characterized by comprising the following steps: mixing o-phenylenediamine and tartaric acid in a proper amount of ethanol solution at room temperature, putting the mixture into an ultrasonic cleaner for ultrasonic treatment for a certain time, then putting the mixture on a magnetic stirrer for stirring for a certain time, after the o-phenylenediamine and the tartaric acid are fully dissolved, mixing a proper amount of sliced dragon bone into the three-component mixed solution, and stirring for a certain time to prepare a four-component mixed solution; transferring the four-component mixed solution into a reaction bottle, reacting for a period of time at 175-185 ℃, and naturally cooling to room temperature to obtain a dark purple solid-liquid mixture; and removing liquid from the dark purple solid-liquid mixture by using an organic filter membrane to leave the dyed hairtail, washing the solution remained on the hairtail for a plurality of times by using ethanol, and drying to obtain the purple hairtail.
The preparation method of the purple Spiraria natans based on the special dye is characterized in that o-phenylenediamine and tartaric acid are mixed in 10-20 ml of ethanol solution according to the mass ratio of 100:100 mg.
The preparation method of the purple dragon silk based on the special dye is characterized in that the aperture size of the organic filter membrane is 0.3-0.6 micron.
The preparation method of the purple Spiraria natans based on the special dye is characterized in that the stirrer is a magnetic stirrer.
The preparation method of the purple Spiraria natans based on the special dye is characterized in that the purple Spiraria natans is placed on a stirrer and stirred for a certain time of 30-60 minutes.
The preparation method of the purple dragon silk based on the special dye is characterized in that a proper amount of dragon silk is mixed in the solution and stirred for a period of 30-60 minutes.
The preparation method of the purple dragon silk based on the special dye is characterized in that a proper amount of the dragon silk is mixed in the solution, and the amount ratio of the dragon silk to the o-phenylenediamine is 1: 1-2.
The preparation method of the purple dragon silk based on the special dye is characterized in that the ultrasonic treatment is carried out for a period of 10-20 minutes.
The preparation method of the purple Spiraria natans based on the special dye is characterized by reacting for 12-15 hours at 175-185 ℃.
The invention has the following beneficial technical effects: (1) the adopted dragon silk is green, environment-friendly and renewable, has low cost, no toxicity, no pollution, easy modification and biocompatibility, and can be applied to large-scale production; (2) the invention uses one pot of solvent thermal reaction to self-assemble to form covalent bond, the prepared special dye is stable and does not coagulate, and the preparation process is simple to operate; (3) the purple dragon silk obtained by the invention is a novel ultraviolet dragon silk which is uniform in color and stable in structure and is based on a special dye and formed by a chemical reaction between the special dye and the dragon silk; (4) the purple dragon yarn based on the special dye has good biocompatibility, comprehensively utilizes the advantages of the special dye and the dragon yarn, can be applied to the fields of information encryption, green dyeing and finishing and the like, and widens the application range of dyeing materials.
Drawings
Fig. 1 is a macroscopic view of a novel purple dragon yarn based on a specific dye.
Fig. 2 is a microscopic view of a novel purple Spiraria filament based on a specific dye.
FIG. 3 is a diagram of the UV-VIS absorption spectrum of a novel purple hairspring based on a special dye.
Detailed Description
The technology of the present invention is further illustrated below with reference to specific examples.
First, an embodiment is described.
A preparation method of purple Spiraria filament based on special dye comprises the following steps:
1. mixing o-phenylenediamine and tartaric acid (the mass ratio is 100mg:100 mg) in 10-20 mL of ethanol solution at room temperature, putting the three-component mixed solution into an ultrasonic cleaner for ultrasonic treatment for 10-20 minutes, then putting the ultrasonic cleaner on a magnetic stirrer for stirring for 30-60 minutes, and after the o-phenylenediamine and the tartaric acid are fully dissolved, mixing the dried dragons (100 mg-200 mg) in the three-component mixed solution and stirring for 30-60 minutes to obtain a four-component mixed solution.
2. And transferring the four-component mixed solution into a 25mL reaction bottle, and placing the reaction bottle at 175-185 ℃ for reaction for 12-15 hours to obtain a deep purple solid-liquid mixture.
3. Removing liquid from the deep purple solid-liquid mixture by using a 0.3-0.6 micron organic filter membrane, leaving dyed hairline, washing the solution remained on the hairline for a small number of times (5-10 mL and 5-8 times) by using a solvent component ethanol, then drying the solution in a forced air drying oven at 50-80 ℃, and storing the obtained purple hairline in a dryer in a dark place.
Second, embodiment two.
A preparation method of purple Spiraria filament based on special dye comprises the following steps:
1. at room temperature, firstly, o-phenylenediamine and tartaric acid (the mass ratio is 100mg:100 mg) are mixed in 15mL of ethanol solution, then the mixed solution is placed in an ultrasonic cleaner for ultrasonic treatment for 15 minutes, then the ultrasonic cleaner is placed on a magnetic stirrer for stirring for 40 minutes, after the o-phenylenediamine and the tartaric acid are fully dissolved, 100mg of dragon silk is mixed in the three-component mixed solution and stirred for 40 minutes, and a four-component mixed solution is prepared.
2. Transferring the four-component mixed solution into a 25mL reaction bottle, placing the reaction bottle at 175 ℃ for reaction for 12 hours, and naturally cooling to obtain a dark purple solid-liquid mixture.
3. Removing liquid from the dark purple solid-liquid mixture by using a 0.3 micron organic filter membrane, leaving dyed dragon silk, cleaning the solution remained on the dragon silk by using ethanol for a small number of times (5-10 mL, 5-8 times), and then drying in a forced air drying oven at 50 ℃ to obtain the purple dragon silk.
And III, embodiment III.
A preparation method of purple Spiraria filament based on special dye comprises the following steps:
1. at room temperature, firstly, o-phenylenediamine and tartaric acid (the mass ratio is 100mg:100 mg) are mixed in 20mL of ethanol solution, then the mixed solution is placed in an ultrasonic cleaner for ultrasonic treatment for 20 minutes, then the mixed solution is placed on a magnetic stirrer for stirring for 60 minutes, after the o-phenylenediamine and the tartaric acid are fully dissolved, 150mg of dragon silk is mixed in the three-component mixed solution and stirred for 60 minutes, and a four-component mixed solution is prepared.
2. And transferring the four-component mixed mixture into a 25mL reaction bottle, placing the reaction bottle at 180 ℃ for reacting for 15 hours, and naturally cooling to obtain a dark purple solid-liquid mixture.
3. And removing liquid from the dark purple solid-liquid mixture by using a 0.45-micron organic filter membrane to leave dyed dragon filaments, washing the solution remained on the dragon filaments for a small number of times (5-10 mL, 5-8 times) by using ethanol, and drying in a forced air drying oven at 70 ℃ to obtain the purple dragon filaments.
Fourth, the fourth embodiment.
A preparation method of purple Spiraria filament based on special dye comprises the following steps:
1. at room temperature, firstly, o-phenylenediamine and tartaric acid (the mass ratio is 100mg:100 mg) are mixed in 20mL of ethanol solution, then the mixed solution is placed in an ultrasonic cleaner for ultrasonic treatment for 15 minutes, then the mixed solution is placed on a magnetic stirrer for stirring for 60 minutes, after the o-phenylenediamine and the tartaric acid are fully dissolved, 200mg of dragon silk is mixed in the three-component mixed solution and stirred for 60 minutes to prepare a four-component mixed solution.
2. Transferring the four-component mixed solution into a 25mL reaction bottle, placing the reaction bottle at 185 ℃ for reacting for 12 hours, and naturally cooling to obtain a dark purple solid-liquid mixture.
3. Removing liquid from the dark purple solid-liquid mixture by using a 0.6 micron organic filter membrane, leaving dyed dragon silk, cleaning the solution remained on the dragon silk by using ethanol for a small number of times (5-10 mL, 5-8 times), and drying in a forced air drying oven at 80 ℃ to obtain the purple dragon silk.
Fifthly, the novel purple dragon hair prepared by the second to fourth comparative examples has uniform and stable color along with the increase of the dosage of the original color dragon hair. It is noted that the color of the dragon filaments did not change significantly over the temperature range used in the examples.
Claims (9)
1. A preparation method of purple Spiraria natans based on special dyes is characterized by comprising the following steps: mixing o-phenylenediamine and tartaric acid in a proper amount of ethanol solution at room temperature, putting the mixture into an ultrasonic cleaner for ultrasonic treatment for a certain time, then putting the mixture on a magnetic stirrer for stirring for a certain time, after the o-phenylenediamine and the tartaric acid are fully dissolved, mixing a proper amount of sliced dragon bone into the three-component mixed solution, and stirring for a certain time to prepare a four-component mixed solution; transferring the four-component mixed solution into a reaction bottle, reacting for a period of time at 175-185 ℃, and naturally cooling to room temperature to obtain a dark purple solid-liquid mixture; and removing liquid from the dark purple solid-liquid mixture by using an organic filter membrane to leave the dyed hairtail, washing the solution remained on the hairtail for a plurality of times by using ethanol, and drying to obtain the purple hairtail.
2. A preparation method of purple dragon silk based on special dye according to claim 1, characterized in that o-phenylenediamine and tartaric acid are mixed in 10-20 ml of ethanol solution according to the mass ratio of 100:100 mg.
3. The method for preparing purple dragon silk based on special dye according to claim 1, wherein the aperture size of the organic filter membrane is 0.3-0.6 micron.
4. The method for preparing purple dragon silk based on special dyes according to claim 1, wherein the stirrer is a magnetic stirrer.
5. The preparation method of purple dragon silk based on special dye according to claim 1, characterized in that the purple dragon silk is placed on a stirrer to be stirred for a certain time of 30-60 minutes.
6. A preparation method of purple dragon silk based on special dye according to claim 1, characterized in that a proper amount of dragon silk is mixed in the solution and stirred for a period of 30-60 minutes.
7. The method for preparing purple dragon silk based on special dye according to claim 1, wherein a proper amount of dragon silk is mixed in the solution, and the amount ratio of the dragon silk to the o-phenylenediamine is 1: 1-2.
8. The preparation method of purple dragon silk based on special dye according to claim 1, characterized in that the ultrasonic treatment is performed for a period of 10-20 minutes.
9. The preparation method of purple dragon yarn based on special dye according to claim 1, characterized in that the reaction is carried out at 175-185 ℃ for 12-15 hours.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110150568.1A CN113529435B (en) | 2021-02-04 | 2021-02-04 | Preparation method of purple natatorium yarn based on special dye |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110150568.1A CN113529435B (en) | 2021-02-04 | 2021-02-04 | Preparation method of purple natatorium yarn based on special dye |
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| CN113529435A true CN113529435A (en) | 2021-10-22 |
| CN113529435B CN113529435B (en) | 2023-04-28 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB455274A (en) * | 1935-04-10 | 1936-10-12 | Chem Ind Basel | Production of fast tints on cellulosic fibres |
| FR1203681A (en) * | 1957-03-26 | 1960-01-20 | Ciba Geigy | Process for preparing dyed viscose articles |
| CN105350345A (en) * | 2015-11-26 | 2016-02-24 | 青岛大学 | Ionic liquid dyeing method of reactive dyes |
| CN107142748A (en) * | 2017-07-03 | 2017-09-08 | 吴江市意胜纺织有限公司 | Fade-proof textile dyestuff of a kind of antibacterial and preparation method thereof |
-
2021
- 2021-02-04 CN CN202110150568.1A patent/CN113529435B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB455274A (en) * | 1935-04-10 | 1936-10-12 | Chem Ind Basel | Production of fast tints on cellulosic fibres |
| FR1203681A (en) * | 1957-03-26 | 1960-01-20 | Ciba Geigy | Process for preparing dyed viscose articles |
| CN105350345A (en) * | 2015-11-26 | 2016-02-24 | 青岛大学 | Ionic liquid dyeing method of reactive dyes |
| CN107142748A (en) * | 2017-07-03 | 2017-09-08 | 吴江市意胜纺织有限公司 | Fade-proof textile dyestuff of a kind of antibacterial and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 张建英: "活性染料在印花中的应用及研究进展情况", 《印染助剂》 * |
| 银鹏 等: "微晶纤维素表面接枝对苯二胺的制备及其荧光性能", 《材料导报》 * |
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