Preparation method of modified thymol-based bio-based repairing agent for polyester dyeing

Abstract

The invention relates to the field of textile auxiliaries, and discloses a preparation method of a modified thymol-based bio-based repairing agent for polyester dyeing, which comprises the following steps: reacting thymol with benzoyl chloride to prepare a benzoic acid thymol ester intermediate; the repairing agent for dyeing polyester fabrics is obtained by compounding cardanol polyoxyethylene ether sulfonate according to a certain ratio. The bio-based repairing agent prepared by the invention can improve the dispersity, low-temperature dyeing property and migration property of disperse dye, and effectively solves the problem of textile waste caused by dyeing defects and uneven dyeing in the actual process.

Description

Technical Field

[0001] The invention relates to the field of textile auxiliaries, and in particular to a method for preparing a bio-based mending agent based on modified thymol for polyester dyeing. Background Art

[0002] As an important synthetic fiber, polyester is widely used in the textile industry. Polyester fiber has many advantages such as light weight, high strength, good elasticity, good wear resistance, mildew resistance and moth resistance, which makes it the preferred material in many textile manufacturing. However, the polyester dyeing process is a relatively complex and problem-prone link. The traditional polyester dyeing process is usually carried out in an acidic environment of 130-140℃ using disperse dyes. Disperse dyeing of polyester is generally divided into two processes. First, the disperse dye approaches the fiber from the dye solution and adsorbs on the fiber surface. Then, as the temperature gradually increases and reaches the glass transition temperature of the polyester fiber, the dye slowly diffuses into the fiber. As the temperature rises, the proportion of the amorphous region of the polyester fiber gradually increases, the dye enters the amorphous region and fixes on the fiber, and no longer redistributes, so it is easy to cause irreparable color spots, color flowers, color differences and other defects in the polyester fiber. These defects not only affect the appearance quality of the textiles, but also may cause the product to fail to be genuine, thereby causing great waste of textiles and affecting the economic benefits of the enterprise. Summary of the invention

[0003] The purpose of the present invention is to provide a bio-based repair agent for polyester dyeing, which can make the defects such as color spots, color patterns, color differences, etc. produced in the normal dyeing process of polyester achieve the purpose of uniform color and consistent hue of the fabric in the same treatment process; in addition, the bio-based repair agent is non-toxic and harmless, and can be naturally degraded after use, which reduces the difficulty of printing and dyeing wastewater treatment and reduces the treatment cost, and is environmentally friendly.

[0004] In order to achieve the above object, the present invention adopts the following technical scheme, which is proportioned by mass: A: Add 500-510 parts of thymol and 500-510 parts of benzoyl chloride into a reaction vessel equipped with a condensing reflux device, start stirring, fill with nitrogen, heat to 60-70°C, react for 0.5-1 hour, then gradually raise the temperature to 100-110°C and keep warm for 1-2 hours to obtain thymol benzoate, the reaction formula is as follows:

[0005] B: 20-30 parts of thymol benzoate, 35-50 parts of castor oil polyoxyethylene ether, 10-15 parts of cardanol polyoxyethylene ether sulfonate, and 10-15 parts of solvent are added to a reaction container, stirring is started, and after stirring for 0.5-1 hour, 10-15 parts of deionized water are slowly added, and stirring is continued for 0.5-1 hour to obtain a bio-based repair agent for polyester dyeing.

[0006] Preferably, the average number of polyoxyethylene segments (EO) in the molecular structure of the castor oil polyoxyethylene ether is 10-20.

[0007] Preferably, the average number of polyoxyethylene segments (EO) in the molecular structure of the cardanol polyoxyethylene ether sulfonate is 5 to 12.

[0008] The solvent is one of isopropanol, ethylene glycol monobutyl ether and diethylene glycol monobutyl ether.

[0009] Due to the application of the above technical solution, the present invention has the following advantages: The present invention adopts thymol as raw material to prepare thymol benzoate. Compared with benzyl benzoate, the structure has an isopropyl group at the ortho position of the benzene ring and a methyl group at the meta position, which increases its hydrophobicity and increases its electron cloud density, so that it has a stronger affinity for polyester, interacts with polyester fiber molecules through van der Waals force, can be better combined with the fiber, has a stronger plasticizing effect on polyester, can effectively reduce the glass transition temperature of polyester, enhance the swelling property of the fiber, and strengthen the movement of the fiber molecular chain segment in the amorphous region; in addition, castor oil polyoxyethylene ether and cardanol polyoxyethylene ether sulfonate have a good solubilizing effect on disperse dyes, and can enhance the dispersibility of dyes; the composite synergistic system formed by the three can make disperse dyes migrate more easily from the inside of the fiber to the outside of the fiber, and gradually increase the trend of disperse dye "desorption" as the dyeing temperature increases, so as to realize the rearrangement of disperse dyes in polyester fiber, and achieve the effect of repairing and leveling. Thymol is a bio-based raw material, biodegradable and environmentally friendly.

[0010] Example method The present invention is further described below by means of specific embodiments. In the examples and comparative examples, the average number of polyoxyethylene segments (EO) in the molecular structure of castor oil polyoxyethylene ether is 15, and the average number of polyoxyethylene segments (EO) in the molecular structure of cardanol polyoxyethylene ether sulfonate is 8.

[0011] Example 1 A: Add 500 kg of thymol and 500 kg of benzoyl chloride into a reaction vessel equipped with a condensing reflux device, start stirring, fill with nitrogen, heat to 60°C, react for 0.5 hour, then gradually increase the temperature to 110°C and keep warm for 2 hours to obtain thymol benzoate.

[0012] B: Add 20 kg of thymol benzoate, 45 kg of castor oil polyoxyethylene ether, 15 kg of cardanol polyoxyethylene ether sulfonate, and 10 kg of solvent into a reaction container, start stirring, and slowly add 10 kg of deionized water after stirring for 0.5 hour, and stir for 0.5 hour to obtain a bio-based repair agent.

[0013] Example 2 A: Add 505 kg of thymol and 510 kg of benzoyl chloride into a reaction vessel equipped with a condensing reflux device, start stirring, fill with nitrogen, heat to 65°C, react for 0.75 hours, then gradually increase the temperature to 100°C and keep the reaction for 1.5 hours to obtain thymol benzoate.

[0014] B: Add 25 kg of thymol benzoate, 40 kg of castor oil polyoxyethylene ether, 15 kg of cardanol polyoxyethylene ether sulfonate, and 10 kg of solvent into a reaction container, start stirring, stir for 0.75 hours, slowly add 10 kg of deionized water, and stir for 1 hour to obtain a bio-based repair agent.

[0015] Example 3 A: Add 510 kg of thymol and 505 kg of benzoyl chloride into a reaction vessel equipped with a condensing reflux device, start stirring, fill with nitrogen, heat to 70°C, react for 1 hour, then gradually increase the temperature to 105°C and keep the temperature for 1 hour to obtain thymol benzoate.

[0016] B: Add 30 kg of thymol benzoate, 35 kg of castor oil polyoxyethylene ether, 15 kg of cardanol polyoxyethylene ether sulfonate, and 10 kg of solvent into a reaction container, start stirring, stir for 1 hour, slowly add 10 kg of deionized water, and stir for 0.75 hour to obtain a bio-based repair agent.

[0017] Comparative Example 1 Add 20 kg of benzyl benzoate, 45 kg of castor oil polyoxyethylene ether, 15 kg of cardanol polyoxyethylene ether sulfonate, and 10 kg of solvent into a reaction container, start stirring, stir for 0.5 hour, then slowly add 10 kg of deionized water and stir for 1 hour.

[0018] Application evaluation process: Transferability Disperse Violet HFRL 2.0% Dye bath pH 4.5~5 Repair agent dosage 1.0 g / L Bath ratio 1:10 Heating rate: 2.0℃ / min Dyeing temperature 130℃ Staining time 30 min The migration test was carried out in accordance with the industry standard HG / T4263-2011 "Determination of migration properties of textile dyeing and finishing auxiliaries and polyester leveling agents", and the blank control was without adding repair agent. The results are shown in Table 1.

[0019] Table 1 Comparison of migration test results

[0020] Low temperature dyeability Disperse dark blue HGL 1.0% Dye bath pH 4.5~5 Repair agent dosage 1.0 g / L Bath ratio 1:10 Heating rate: 2.0℃ / min Dyeing temperature 90~130℃ Staining time 30 min The above dyeing process was used to test the color depth (K / S value) at 90, 100, 110, and 130°C. The blank control was a sample without adding a repairing agent. The results are shown in Table 2.

[0021] Table 2 Comparison of low temperature staining results

[0022] Dispersibility According to the industry standard HG / T 4261-2011 "Determination of High-temperature Dispersibility of Leveling Agents for Textile Dyeing and Finishing Auxiliary Products", the working solution was prepared according to the process formula, and the temperature was raised to 130°C at 2°C / min, and then cooled to 90°C after insulation. Two layers of filter paper were stacked and placed in a Büchner funnel, and the vacuum pump was turned on. The working solution was poured into the funnel while hot for filtration. After the working solution had all flowed down, the filter paper was taken out, and the filter paper was naturally dried and rated according to the color depth of the filter paper surface. The results are shown in Table 3.

[0023] Table 3 Comparison of dispersion test results

[0024] From the results in Table 1 to Table 3, it can be found that the transfer performance of the embodiment is significantly improved compared with the blank of the comparative example, and the transfer performance of the embodiment is better than that of the comparative example, indicating that the embodiment has good transfer performance; the K / S of 110°C low-temperature dyeing without adding an auxiliary agent is only 8.32, while the embodiment reaches more than 10, indicating that the low-temperature dyeing performance of the embodiment is good, which also means that the embodiment has good plasticizing performance; when no auxiliary agent is added, the dispersibility of the two disperse dyes is level 2, and after adding the example and the comparative example, the dispersibility reaches level 5, indicating that the embodiment has good dye dispersibility. In short, the embodiment has good low-temperature dyeing and transfer performance, which also shows that it has good color stain repair performance.

[0025] The technical scope of the present invention is not limited to the contents in the above description. Those skilled in the art can make various deformations and modifications to the above embodiments without departing from the technical concept of the present invention, and these deformations and modifications should all fall within the scope of the present invention.

Claims

1. A method for preparing a bio-based repair agent based on modified thymol for polyester dyeing, wherein the following is prepared by proportioning by mass, characterized in that The method and steps include: (1) Add 500-510 parts of thymol and 500-510 parts of benzoyl chloride to a reaction vessel equipped with a condensing reflux device, start stirring, fill with nitrogen, heat to 60-70°C, react for 0.5-1 hour, then gradually increase the temperature to 100-110°C and keep warm for 1-2 hours to obtain thymol benzoate; (2) Add 20-30 parts of thymol benzoate, 35-50 parts of castor oil polyoxyethylene ether, 10-15 parts of cardanol polyoxyethylene ether sulfonate and 10-15 parts of solvent to a reaction vessel, start stirring, stir for 0.5-1 hour, then slowly add 10-15 parts of deionized water, stir for 0.5-1 hour to obtain a bio-based repair agent for polyester dyeing.

2. According to claim 1, a method for preparing a bio-based repair agent based on modified thymol for polyester dyeing, wherein in step (2), the average number of polyoxyethylene segments (EO) in the molecular structure of castor oil polyoxyethylene ether is 10-20, the average number of polyoxyethylene segments (EO) in the molecular structure of cardanol polyoxyethylene ether sulfonate is 5-12, and the solvent is one of isopropanol, ethylene glycol monobutyl ether, and diethylene glycol monobutyl ether.

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