A high temperature levelling agent and a method for its preparation

Abstract

The application discloses a high-temperature level dyeing agent and a preparation method thereof. Components of the high-temperature level dyeing agent include 10-20 parts of glycerol ether oleic acid ester, 8-15 parts of polyethylene glycol dioleic acid ester, 8-10 parts of dodecyl benzene sulfonic acid, 5-15 parts of castor oil polyoxyethylene ether, 3-6 parts of 2-ethylhexyl sulfate sodium salt, 1-2 parts of sodium hydroxide, 5-15 parts of maleic anhydride polyethylene glycol ester-acrylic acid copolymer, 10-20 parts of ethanol and 20-30 parts of deionized water. The application has excellent dyeing retarding property, dyeing migration property, dispersing property and permeating property, can emulsify and disperse residual oil in fibers, has good chelating capacity for metal ions in a dye bath, has strong applicability to dyeing conditions, is suitable for various complex conditions when used for polyester fiber dyeing, has good level dyeing property, and can effectively prevent color mottle, color spot, color point, color lightness and color fading.

Description

[Technical Field]

[0001] This invention relates to the field of textile technology, specifically to a high-temperature leveling agent and its preparation method. [Background Technology]

[0002] Polyester is the most produced synthetic fiber, widely used in textiles such as clothing, bedding, and decorative fabrics. Polyester fibers are mainly dyed with disperse dyes. During high-temperature and high-pressure dyeing, due to the poor dispersibility and leveling properties of disperse dyes, and because polyester is a hydrophobic fiber with a tightly packed molecular structure, the dye does not easily penetrate the fiber interior. Therefore, high-temperature resistant leveling agents are often added to promote uniform dyeing.

[0003] See the invention patent application with patent number 202211043984.2, which discloses a bio-based high-temperature leveling agent, its preparation method, and its application. The technical solution involves: first, adding bio-based organic fatty acids to the reaction. Then, sodium lignin sulfonate is added to the final product. This is an excellent anionic surfactant, obtained by sulfonating lignin to convert it into sodium sulfonate salt. It can solve the problem of dye agglomeration and staining caused by the low cloud point of nonionic surfactants. The synergistic and enhancing effects of nonionic and anionic surfactants are utilized to formulate a high-performance bio-based high-temperature leveling agent that improves the leveling effect of fabrics.

[0004] As described above, most polyester high-temperature leveling agents currently on the market are compound products of nonionic and anionic surfactants. These leveling agents mainly utilize the synergistic effect of the slow-dyeing and migration properties of nonionic surfactants and the dispersing properties of anionic surfactants to achieve a leveling effect on disperse dyes on polyester fibers. However, in actual production, many factors affect uniform dyeing, such as the fabric's density, residual oil on the fibers, the presence of polyester oligomers, metal ions in the water, and the characteristics of the dye itself. These factors can easily lead to defects such as color spots, stains, and discoloration on the dyed fabric even when leveling agents are added. At the same time, in order to increase the dispersibility of dyes, traditional leveling agent formulations usually add a large amount of aromatic sulfonate anionic surfactants as dispersants. At high temperatures, these dispersants can easily cause certain groups of disperse dyes to undergo reduction reactions, resulting in light color and color change, especially for bright colors, where the dyed fabric becomes noticeably dull.

[0005] In view of the shortcomings of current high-temperature leveling agents, the inventors propose the following technical solution. [Summary of the Invention]

[0006] The technical problem to be solved by the present invention is to overcome the shortcomings of the prior art and provide a high-temperature leveling agent and its preparation method.

[0007] To solve the above-mentioned technical problems, the present invention adopts the following technical solution: a high-temperature leveling agent, wherein the components of the high-temperature leveling agent include, by weight, 10-20 parts of glyceryl ether oleate, 8-15 parts of polyethylene glycol dioleate, 8-10 parts of dodecylbenzene sulfonic acid, 5-15 parts of castor oil polyoxyethylene ether, 3-6 parts of sodium 2-ethylhexyl sulfate, 1-2 parts of sodium hydroxide, 5-15 parts of maleic anhydride polyethylene glycol ester-acrylic acid copolymer, 10-20 parts of ethanol, and 20-30 parts of deionized water.

[0008] Furthermore, in the above technical solution, the high-temperature leveling agent components include, by weight, 17 parts glyceryl ether oleate, 8 parts polyethylene glycol dioleate, 9 parts dodecylbenzene sulfonic acid, 10 parts castor oil polyoxyethylene ether, 4 parts sodium 2-ethylhexyl sulfate, 1.5 parts sodium hydroxide, 10 parts maleic anhydride polyethylene glycol ester-acrylic acid copolymer, 15 parts ethanol, and 25.5 parts deionized water.

[0009] Furthermore, the high-temperature leveling agent preparation method described in the above technical solution includes: Step 1, adding deionized water and ethanol to a reaction vessel and stirring for 5-10 minutes; Step 2, adding dodecylbenzenesulfonic acid and stirring for 10 minutes; Step 3, sequentially adding glyceryl ether oleate, polyethylene glycol dioleate, castor oil polyoxyethylene ether, and sodium 2-ethylhexyl sulfate, stirring for 25-30 minutes after each addition; Step 4, adding dissolved sodium hydroxide and adjusting the pH to 6.5-7.0; Step 5, adding maleic anhydride polyethylene glycol ester-acrylic acid copolymer and stirring for 25-30 minutes; Step 6, after completion, allowing to stand and filtering out the material.

[0010] This invention possesses excellent slow-dyeing, migration, dispersibility, and penetration properties. It also emulsifies and disperses residual oils in fibers and has a good chelating ability for metal ions in the dye bath. It is highly adaptable to various dyeing conditions. When used for dyeing polyester fibers, this invention is suitable for various complex conditions. It is a novel high-temperature leveling agent with good leveling properties, effectively preventing color spots, blemishes, and light or faded colors, thus improving productivity and meeting urgent market demands.

Detailed Implementation Methods

[0011] The present invention will be further described below through specific embodiments.

[0012] Example 1:

[0013] A high-temperature leveling agent, wherein the high-temperature leveling agent is composed of the following components in parts by weight: 10 parts glyceryl ether oleate, 15 parts polyethylene glycol dioleate, 10 parts dodecylbenzene sulfonic acid, 12 parts castor oil polyoxyethylene ether, 6 parts sodium 2-ethylhexyl sulfate, 1.7 parts sodium hydroxide, 5 parts maleic anhydride polyethylene glycol ester-acrylic acid copolymer, 18 parts ethanol, and 22.3 parts deionized water.

[0014] The preparation process is as follows:

[0015] Step 1: Add deionized water and ethanol to the reaction vessel and stir for 10 minutes;

[0016] Step 2: Add dodecylbenzenesulfonic acid and stir for 10 minutes;

[0017] Step 3: Add glyceryl ether oleate, polyethylene glycol dioleate, castor oil polyoxyethylene ether, and sodium 2-ethylhexyl sulfate in sequence, stirring for 25 minutes after each addition;

[0018] Step 4: Add the dissolved sodium hydroxide and adjust the pH to 6.5-7.0;

[0019] Step 5: Add maleic anhydride polyethylene glycol ester-acrylic acid copolymer and stir for 25 minutes;

[0020] Step 6: After completion, let stand, filter and discharge to obtain the high-temperature leveling agent of the present invention.

[0021] Example 2:

[0022] Example 2: High-Temperature Leveling Agent. This high-temperature leveling agent is composed of the following components in parts by weight: 10 parts glyceryl ether oleate, 15 parts polyethylene glycol dioleate, 8 parts dodecylbenzene sulfonic acid, 6 parts castor oil polyoxyethylene ether, 3 parts sodium 2-ethylhexyl sulfate, 1.3 parts sodium hydroxide, 15 parts maleic anhydride polyethylene glycol ester-acrylic acid copolymer, 12 parts ethanol, and 29.7 parts deionized water. The preparation method is basically the same as in Example 1.

[0023] Example 3:

[0024] Example 3: High-Temperature Leveling Agent. This high-temperature leveling agent is composed of the following components in parts by weight: 17 parts glyceryl ether oleate, 8 parts polyethylene glycol dioleate, 9 parts dodecylbenzene sulfonic acid, 10 parts castor oil polyoxyethylene ether, 4 parts sodium 2-ethylhexyl sulfate, 1.5 parts sodium hydroxide, 10 parts maleic anhydride polyethylene glycol ester-acrylic acid copolymer, 15 parts ethanol, and 25.5 parts deionized water. The preparation method is basically the same as in Example 1.

[0025] Performance testing

[0026] Using the high-temperature leveling agent sample provided by the dyeing plant as a comparative example, the application performance of the high-temperature leveling agents obtained by compounding the above embodiments was compared and tested.

[0027] (a) Slow-release test

[0028] After degreasing and pre-setting treatment, polyester knitted fabric is dyed according to the following formula and process:

[0029]

[0030]

[0031] Bath ratio = 1:20

[0032] 130℃×30min

[0033] During the dyeing process, one fabric sample was taken at each of the following temperatures: 90℃, 100℃, 110℃, 120℃, 130℃, and 130℃ for 30 minutes. The samples were then washed, reduced-washed, washed again, and dried. After the fabric samples cooled and regained moisture, the color depth of the test fabric sample at each temperature was measured relative to the blank sample (100%) using a Datacolor colorimeter. The results are as follows:

[0034]

[0035] In the initial stage of polyester fiber dyeing, whether the dye can be slowly and evenly adsorbed on the fiber surface has a significant impact on the uniformity of dyeing. When the glass transition temperature of polyester is reached at around 110°C, the dyeing rate increases rapidly with increasing temperature. This is the key stage for the leveling agent to fully exert its dispersing, retarding, and migration effects. The above results show that the retarding effect of each embodiment of the present invention is better than that of the comparative example, and the impact on the final color yield is very small.

[0036] (II) Migration test:

[0037] After degreasing, 100% polyester knitted fabric is dyed according to the following process:

[0038] 4.0% Dispersible Black ECT

[0039] 0.5g / L glacial acetic acid

[0040] Bath ratio = 1:20

[0041] 130℃×45min

[0042] Then, weigh equal amounts of the dyed fabric sample (after reduction washing and drying) and the undyed fabric (white fabric), and place them in the following dye bath for transfer dyeing treatment:

[0043] x g / L leveling agent (x = 0, 1.0, where 0 is the blank sample)

[0044] 0.5g / L glacial acetic acid

[0045] Bath ratio = 1:20

[0046] 130℃×45min

[0047] The dyed fabric samples underwent washing, reduction cleaning, washing, and drying. After the fabric samples cooled and regained moisture, the color depth (%) of the dyed fabric sample before transfer was measured relative to the original color depth (100%) using a Datacolor colorimeter, comparing the white fabric after transfer and the dyed fabric after transfer. The results are as follows:

[0048]

[0049] As can be seen from the above results, the migration rate of each embodiment of the present invention is higher than that of the comparative example. In the process of dyeing polyester fibers with disperse dyes, the leveling agent with good migration performance has a good migration ability to the dyes that are not uniformly adsorbed in the early stage of dyeing, thereby effectively preventing the generation of color spots and discoloration.

[0050] (III) High Temperature Dispersibility

[0051] Prepare 100ml of the following working solution and process it in a staining machine at 130℃ for 30min. Then cool it to 70℃ and perform vacuum filtration. Record the time for vacuum filtration with a stopwatch. Then remove the upper filter paper and let it air dry naturally.

[0052] 0.1 g / L Dispersible Deep Blue H-GL

[0053] x g / L leveling agent (x = 0, 0.5, where 0 is the blank sample)

[0054] 0.5g / L glacial acetic acid

[0055] Observe and rate the residual dye on the dried filter paper. No dye aggregation is grade 5, slight dye particles are grade 4, dye particles are grade 3, obvious dye aggregation is grade 2, and very obvious dye aggregation is grade 1.

[0056] The results are as follows:

[0057] blank sample Example 1 Example 2 Example 3 Comparison sample Filtration time 13〞44 10〞92 10〞67 10〞73 11〞58 Filter paper rating 1-2 4-5 5 5 3

[0058] The shorter the filtration time, the better the dispersibility. As can be seen from the table above, the filtration time in each embodiment of the present invention is faster than that of the control sample, indicating that the dye is well dispersed in the test solution of the embodiments.

[0059] The amount of dye residue on the filter paper after filtration is another reliable method for assessing the apparent dispersibility of the sample. Less dye residue on the filter paper results in a higher rating, indicating better sample dispersibility. As can be seen from the rating results in the table above, there is virtually no dye particle residue on the filter paper of the embodiments of this invention, while the control sample has a small amount of dye particles on its filter paper, indicating that the dispersibility of the embodiments is better than that of the control sample.

[0060] In summary, the high-temperature leveling agents prepared in the various embodiments of the present invention have good high-temperature dispersion stability and can effectively prevent the formation of color spots when used for high-temperature and high-pressure dyeing of polyester with disperse dyes.

[0061] (iv) Experiment on the effect on the color of dyeing

[0062] 0.05% Disperse Brilliant Blue SR

[0063] x g / L leveling agent (x = 0, 0.5, where 0 is the blank sample)

[0064] 0.5g / L glacial acetic acid

[0065] Bath ratio = 1:20

[0066] 130℃×30min

[0067] After the fabric samples dyed according to the above formula and process were washed, dried, and naturally cooled to regain moisture, the color depth and color difference of each fabric sample relative to the blank sample were measured using a Datacolor colorimeter, with the blank sample as the standard. The results are shown in the table below:

[0068] Example 1 Example 2 Example 3 Comparison sample blank sample Color depth 97.09 98.83 99.02 92.58 100 Total color difference DE 0.27 0.16 0.12 0.64 0 Visual inspection Slightly lighter and darker Approximate blank sample Approximate blank sample Lighter than darker bright

[0069] As can be seen from the results in the table above, the color results of each embodiment are significantly improved compared with the control sample. In particular, the color and depth of the color obtained in Embodiments 2 and 3 are very close to those of the blank sample, indicating that the high-temperature leveling agent prepared in each embodiment of the present invention has low decolorization and good color stability. When used for high-temperature and high-pressure dyeing of polyester with disperse dyes, it can effectively avoid the occurrence of light color and color fading.

[0070] Based on an evaluation of the overall performance of slow dyeing, transfer dyeing, high-temperature dispersion, and the degree of influence on the color of the dyed fabric, Example 3 is the preferred option.

[0071] Of course, the above description is only a specific embodiment of the present invention and is not intended to limit the scope of the present invention. All equivalent changes or modifications made to the structure, features and principles described in the claims of the present invention should be included in the scope of the claims of the present invention.

Claims

1. A high-temperature leveling agent, characterized in that: The components of this high-temperature leveling agent, by weight, include: 10-20 parts glyceryl ether oleate, 8-15 parts polyethylene glycol dioleate, 8-10 parts dodecylbenzene sulfonic acid, 5-15 parts castor oil polyoxyethylene ether, 3-6 parts sodium 2-ethylhexyl sulfate, 1-2 parts sodium hydroxide, 5-15 parts maleic anhydride polyethylene glycol ester-acrylic acid copolymer, 10-20 parts ethanol, and 20-30 parts deionized water; Its preparation method includes: Step 1: Add deionized water and ethanol to the reaction vessel and stir for 5-10 minutes; Step 2: Add dodecylbenzenesulfonic acid and stir for 10 minutes; Step 3: Add glyceryl ether oleate, polyethylene glycol dioleate, castor oil polyoxyethylene ether, and sodium 2-ethylhexyl sulfate in sequence, stirring for 25-30 minutes after each addition; Step 4: Add the dissolved sodium hydroxide and adjust the pH to 6.5-7.0; Step 5: Add maleic anhydride polyethylene glycol ester-acrylic acid copolymer and stir for 25-30 minutes; Step 6: After completion, let it stand, then filter and discharge the material.

2. The high-temperature leveling agent according to claim 1, characterized in that: The high-temperature leveling agent comprises, by weight, 17 parts glyceryl ether oleate, 8 parts polyethylene glycol dioleate, 9 parts dodecylbenzene sulfonic acid, 10 parts castor oil polyoxyethylene ether, 4 parts sodium 2-ethylhexyl sulfate, 1.5 parts sodium hydroxide, 10 parts maleic anhydride polyethylene glycol ester-acrylic acid copolymer, 15 parts ethanol, and 25.5 parts deionized water.

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