Low-temperature one-bath dyeing method for apocynum venetum yarns by using saline-alkali soil

By using saline-alkali biosalt and silane coupling agent for low-temperature one-bath dyeing in textile dyeing technology, the problems of high energy consumption, high cost and difficult performance retention in the prior art are solved, and efficient and environmentally friendly dyeing effect is achieved, and the excellent performance of the yarn is retained.

CN119900184APending Publication Date: 2025-04-29XINJIANG UNIVERSITY
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Patent Information

Application Number
CN202510022666.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-01-07
Publication Date
2025-04-29

AI Technical Summary

Technical Problem

The existing textile dyeing technology has high demands in terms of energy consumption and production costs, and it is difficult to effectively retain the antibacterial properties and UV resistance of the yarn.

Method used

The low-temperature one-bath dyeing is performed using saline-alkali biosalt and silane coupling agent. By adjusting the chemical environment of the dyeing system and improving the wettability and adsorption of the yarn surface, the effective combination of dye and fiber is achieved.

Benefits of technology

The dyeing of a low-temperature bath is achieved, reducing energy consumption and production costs, while retaining the antibacterial properties and UV resistance of Robu linen yarn, promoting the progress of textile dyeing technology, and providing a new direction for the comprehensive utilization of saline-alkali land resources.

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Abstract

The invention provides a novel low-temperature constant-temperature dyeing technology for apocynum venetum fibers, traditional high-temperature dyeing is changed into dyeing from 40 DEG C to constant temperature of 60 DEG C, saline-alkali soil biologic salt is used for replacing common accelerating salt in a traditional dyeing process, and an amino silane coupling agent is supplemented to achieve a color fixing effect similar to that of traditional color fixing salt on dye. According to the innovation, the dyeing process is simplified, the energy consumption and the cost are reduced, and ecological improvement and resource reutilization of the saline-alkali soil are promoted. Meanwhile, according to the technology, the color fixing effect and uniformity of the dye are guaranteed while operation errors are reduced, and the double advantages of being green, clean and efficient in production are shown.
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Description

Technical Field

[0001] The invention relates to the technical field of textile dyeing and finishing, in particular to a low-temperature one-bath dyeing method for apocynum yarn with biological salt from saline-alkali land. Background Art

[0002] Saline-alkali land refers to land with high salt and alkali content in the soil. This soil environment has a significant impact on plant growth and crop yields. The special environment of saline-alkali land makes the salt and alkali content in the soil a key factor affecting plant growth. In the dyeing process, the use of biological salts in saline-alkali land may help adjust the pH value, ionic strength and other parameters of the dyeing system, thereby affecting the dyeing performance and dyeing effect of the dye.

[0003] The synergistic effect of saline-alkali land biological salt and silane coupling agent has brought innovation to the low-temperature one-bath dyeing technology of apocynum yarn. This technology uses the unique biological salt in saline-alkali land to adjust the chemical environment of the dyeing system and enhance the penetration of the dye; at the same time, the silane coupling agent, as a high-efficiency auxiliary agent, improves the wettability and adsorption of the yarn surface, making it easier for the dye to combine with the fiber. This innovative method not only simplifies the dyeing process, realizes the completion of dyeing in one bath at low temperature, effectively reduces energy consumption and production costs, but also retains the original excellent properties of apocynum yarn, such as antibacterial and UV resistance. The application of this technology not only helps to promote the advancement of textile dyeing technology, but also provides a new direction for the comprehensive utilization of saline-alkali land resources. Summary of the invention

[0004] In view of the defects of the prior art, the present invention provides a low-temperature one-bath dyeing method for apocynum yarn using saline-alkali land biological salt, which effectively reduces energy consumption and production costs, and also retains the original excellent properties of apocynum yarn, such as antibacterial and anti-ultraviolet capabilities. The application of this technology not only helps to promote the progress of textile dyeing technology, but also provides a new direction for the comprehensive utilization of saline-alkali land resources.

[0005] In order to achieve the above object, the technical solution provided by the present invention is a low-temperature one-bath dyeing method for apocynum yarn using saline-alkali land biological salt, comprising the following steps:

[0006] S100, at room temperature of 25°C, weigh saline-alkali soil and place it in an appropriate amount of distilled water, heat it in a water bath, filter it several times, and dry it to obtain saline-alkali soil biological salt for later use;

[0007] S200, at room temperature of 25°C, completely immersing the impurity-removed apocynum yarn in distilled water at a temperature of 25°C, and wringing out excess water after the yarn is completely wet, so that the yarn is in a semi-dry state for standby use;

[0008] S300, at room temperature 25°C, weigh an appropriate amount of reactive dye and place it in an appropriate amount of distilled water at a temperature of 25°C to prepare a dye solution with a concentration of 100ppm for standby use;

[0009] S400, placing the dye solution at a temperature of 25° C. in S300 into a constant temperature environment at 60° C.;

[0010] S500, adding an appropriate amount of saline-alkali biological salt to the dye solution at a temperature of 25° C. to dissolve it;

[0011] S600, adding an appropriate amount of silane coupling agent to the dye solution at a temperature of 25° C. to make it evenly dispersed;

[0012] S700, when the temperature of the dye solution after fusion rises to 40°C, add the apocynum yarn to make it evenly dispersed;

[0013] S800, when the temperature of the dyeing solution rises to 60℃, the dyeing is carried out at a constant temperature for 4 hours, and then the dyeing is carried out by washing and drying to achieve low-temperature dyeing of the apocynum yarn.

[0014] Furthermore, the biological salt described in step S100 is biological salt extracted from saline-alkali land, and the concentration of the biological salt is 15 g / L.

[0015] Furthermore, the process flow of the biological salt extraction is as follows: weigh an appropriate amount of saline-alkali soil and place it in an appropriate amount of distilled water at a temperature of 25°C, the mass ratio of saline-alkali soil to water is 1:20, heat it to 95°C in a water bath and stir it for 60 minutes, then let it stand and cool at room temperature, filter it three times after the solution is completely separated into upper and lower layers, take the supernatant, centrifuge it once, the speed is 10000r / min, the processing time is 10min, take the supernatant again and place it in a beaker, and treat it at 80°C for 24-48h.

[0016] Furthermore, the amount of the apocynum yarn in step S200 is 2 g.

[0017] Furthermore, in step S300, the dosage of the reactive dye solution is 100 mL, the concentration of the reactive dye solution is 100 ppm, the dyeing dye is 0.5% by weight to the fabric, and the bath ratio is 1:50.

[0018] Furthermore, in step S500, 1.5 g of the saline-alkali land biological salt is added and stirred for 2-3 minutes.

[0019] Furthermore, in step S600, 2.5 mL of the silane coupling agent is added and stirred for 2-3 minutes; the silane coupling agent is an aminosilane coupling agent, and the component of the aminosilane coupling agent is 3-aminopropyltriethoxysilane.

[0020] Furthermore, after all the saline-alkali land biological salt and the silane coupling agent are added to the dye solution in step S700, the solution is stirred for 20 minutes and the temperature is raised to 40°C.

[0021] Furthermore, in step S800, the temperature of the apocynum yarn is raised to 60° C., and the temperature is kept constant for 60 minutes. The apocynum yarn is taken out, washed, and dried.

[0022] Furthermore, the reactive dye in step S300 is reactive orange, and the mass concentration is 0.1%.

[0023] By adopting the above-mentioned technical scheme, the dyeing process of the present application uses saline-alkali land biological salt and aminosilane coupling agent to replace a large amount of reagents such as sodium sulfate and soda ash in the traditional reactive dye dyeing process, thereby reducing the salt pollution and auxiliary agent pollution generated during the dyeing process, and simplifies the traditional complex dyeing process through the low-temperature constant temperature one-bath dyeing method, thereby achieving a clean and efficient dyeing process.

[0024] Preferably, the salt used in the dyeing process is saline-alkali biological salt with a salt concentration of 15 g / L; the process used during dyeing is: add 25°C biological salt and 25°C aminosilane coupling agent to the dye solution at room temperature of 25°C, mix and stir for 30 minutes, then heat to 40°C for dyeing, and then heat to 60°C for dyeing for 4 hours.

[0025] By adopting the above technical scheme and the above biological salt, it is possible to replace the traditional dyeing process and achieve the dyeing promotion effect on the dyeing of apocynum yarn; the saline-alkali soil biological salt can adjust the ion concentration in the dye solution with the help of the various salts it is rich in, adjust the charge interaction between the dye molecules in the dye solution and the yarn, and combine with the hydroxyl groups on the dye to achieve a good dyeing promotion effect.

[0026] Preferably, the aminosilane coupling agent used in the dyeing process is APTES, and the dosage is 25 mL / L; the process used during dyeing is: add 25°C biological salt and 25°C APTES to the dye solution at 25°C at room temperature and stir for 30 minutes, then heat to 40°C for dyeing, and then heat to 60°C for dyeing for 4 hours.

[0027] By adopting the above technical scheme and the above aminosilane coupling agent, it is possible to replace soda ash in the traditional dyeing process and achieve a color fixing effect for the dyeing of apocynum yarn; the aminosilane coupling agent can adjust the pH value of the dyeing by means of its own polyamino structure, and rely on its unique amphiphilic structure to combine with the functional groups on the dye to provide more reaction sites, thereby achieving good dyeing and color fixing effects.

[0028] Preferably, the reactive dye used in the dyeing process is Reactive Orange X-GN, with an amount of 0.01 g; the mass concentration component of the dye is 0.5% Reactive Orange X-GN, whose chemical name is 4-[4-(disulfuryl)amidophenyl]azobiphenyl, which is an orange crystalline powder azo dye rich in hydroxyl groups.

[0029] By adopting the above technical solution and the above dye, a good color fixation effect for dyeing apocynum yarn can be achieved under the synergistic effect of aminosilane coupling agent and biological salt.

[0030] In summary, the present application includes at least one of the following beneficial technical effects:

[0031] 1. In this application, by using saline-alkali land biological salt to replace commonly used dyeing salts such as sodium sulfate, not only can salt pollution be reduced, but also the dyeing effect of the apocynum yarn in the dyeing process can be approximately the same as that of the traditional dyeing process.

[0032] 2. The silane coupling agent used in this application can replace soda ash for apocynum yarn. Firstly, its polyamino structure can adjust the charge in the solution, promote the ionization of dye molecules and make them combine with fibers, and achieve a certain color fixation effect; secondly, its amino group will combine with the hydroxyl group of the dye molecule to make it more firmly combined with the fiber. The two work together to achieve a good color fixation effect on apocynum yarn.

[0033] 3. The biosalt extraction technology used in this application can extract the rich biosalts in saline-alkali soil, which can have a certain improvement effect on the saline-alkali soil and has a certain reference significance for the management of saline-alkali land. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 is a process flow chart of the present invention;

[0035] Figure 2-5 It is an optical photograph of the apocynum yarn after dyeing in Examples 1-4;

[0036] Figure 6-16 This is an optical photograph of the apocynum yarn after dyeing in Comparative Examples 5-15. DETAILED DESCRIPTION

[0037] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the specific embodiments of the present invention are described in detail below in conjunction with the accompanying drawings. In the following description, many specific details are set forth to facilitate a full understanding of the present invention. However, the present invention can be implemented in many other ways different from those described herein, and those skilled in the art can make similar improvements without violating the connotation of the present invention, so the present invention is not limited by the specific embodiments disclosed below.

[0038] Example 1

[0039] S100. At room temperature of 25°C, weigh an appropriate amount of saline-alkali soil and place it in an appropriate amount of distilled water at a temperature of 25°C, with a mass ratio of saline-alkali soil to water of 1:20. Heat in a water bath to 95°C and stir for 60 minutes. Then let it stand and cool at room temperature. After the solution is completely separated into upper and lower layers, filter it three times. Take the supernatant, centrifuge it once at a speed of 10,000 r / min for 10 minutes, take the supernatant again and place it in a beaker, treat it at 80°C for 24-48 hours, and dry it to obtain the saline-alkali soil biological salt for use. The concentration of the extracted saline-alkali land biological salt is 15 g / L.

[0040] S200. At room temperature of 25°C, completely immerse 2g of the impurity-removed apocynum yarn in distilled water at a temperature of 25°C, wring out excess water after it is completely soaked, and keep it in a semi-dry state for use.

[0041] S300. At room temperature of 25°C, weigh an appropriate amount of reactive dye and place it in an appropriate amount of distilled water at a temperature of 25°C to prepare a dye solution with a concentration of 100ppm for use; the amount of reactive dye solution is 100mL, the concentration of reactive dye solution is 100ppm, the dyeing dye is 0.5% to the weight of the fabric, and the bath ratio is 1:50; the reactive dye is reactive orange X-GN, and the mass concentration is 0.1%.

[0042] S400, placing the dye solution at a temperature of 25°C in S300 into a constant temperature environment at 60°C.

[0043] S500, when the temperature of the dye solution after fusion at 25℃ rises to 40℃, add the apocynum yarn and disperse it evenly.

[0044] S600, when the temperature of the dye solution rises to 60°C, the dyeing is carried out at a constant temperature and oscillation for 4 hours, and then the yarn is washed and dried to achieve low-temperature dyeing of the apocynum yarn.

[0045] It should be noted that in this embodiment, the 25°C dye solution placed in a constant temperature environment of 60°C does not contain APTES and biological salt.

[0046] Example 2

[0047] The process is basically the same as that in Example 1, except that in step S400, 5 mL of APTES is added to the dye solution at 25° C., stirred for 2-3 minutes, stirred evenly, and then placed in a 60° C. environment for dyeing. The other steps are the same as those in Example 1.

[0048] Example 3

[0049] The method is basically the same as that in Example 1, except that in step S400, 0.5 g of biological salt is added to the dye solution at 25° C., stirred for 2-3 minutes, stirred evenly, and then placed in an environment at 60° C. for dyeing. The other steps are the same as those in Example 1.

[0050] Example 4

[0051] The method is basically the same as Example 1, except that in step S400, 0.5 g of biological salt is added to the dye solution at 25°C, stirred for 2-3 minutes, and then 5 mL of APTES is added and stirred for 2-3 minutes. After all the dye solution is added, it is stirred for another 20 minutes and placed in a 60°C environment for dyeing. The other steps are the same as Example 1.

[0052] The apocynum yarn of embodiment 1-4 dyeing is as Figure 2-5 As shown in the picture, it can be seen that the apocynum yarn without adding biological salt and APTES and only adding APTES has no obvious color change before and after dyeing, and is almost not dyed; while the apocynum yarn with only adding biological salt has color change before and after dyeing, but its color is lighter than that in Example 4, and there is a big difference.

[0053] The basic conditions and color fastness of the apocynum yarns of Examples 1-4 were tested, and the test results are shown in Table 1.

[0054] The K / S value and color fixation rate of the apocynum yarn of Examples 1-4 were tested, and the test results are shown in Table 2.

[0055] in:

[0056] Colour fastness to rubbing - wet shall be in accordance with GB / T 42223-2022.

[0057] Colour fastness to rubbing - dry shall be in accordance with GB / T 42223-2022.

[0058] Color fastness to light shall be in accordance with GB / T 8427-2019.

[0059] Color fastness to soap washing shall be in accordance with GB / T3921-2008

[0060] The colour fastness to perspiration shall be in accordance with GB / T 3922-2013.

[0061] The Kubelka-Munk law is used to consider the levelness of the dyed yarn. The specific method is as follows: the dyed yarn is evenly wound on a black test plate and three points are randomly selected on it. The three apparent color depths K / S values ​​within the maximum absorption wavelength range are measured three times using a colorimeter. The average value of each K / S value is taken, and the color depth difference is obtained by subtracting the minimum value from the maximum value ( △K / S value) is used to indicate the levelness of the fabric. △ The smaller the K / S value, the better the levelness.

[0062] The specific test data are shown in Table 2. The percentage of dye reacted by the yarn to the mass percentage of dyed dye is the fixation rate. The K / S value of dyed apocynum fabric before and after soaping under different processes was determined by a computer colorimeter, and the fixation rate F of dyed apocynum yarn was calculated according to the formula.

[0063]

[0064] Where: (K / S)1--K / S value after soaping;

[0065] (K / S)0--K / S value before soaping.

[0066] Table 1

[0067] Colour fastness to rubbing - dry Colour fastness to rubbing - wet Color fastness to light Color fastness to soap washing Color fastness to perspiration Example 3 5 4-5 5 3-4 5 Example 4 5 4-5 5 3 5

[0068] By controlling whether APTES (3-aminopropyltriethoxysilane) and biological salts are used in the dyeing process, their effects on the dyeing effect of apocynum yarn are analyzed. Figure 2-5 As shown in Table 1, the yarns of Example 1 and Example 2 are almost not colored after dyeing, so it is meaningless to test the color fastness of these samples, so these samples were not tested for color fastness. Further observation of the data of Example 3 and Example 4 in Table 1 shows that the color fastness test results of the two are similar. Except for the soap fastness, the other fastness test results all reach level 4-5 and above, and the soap fastness also reaches the minimum requirement of level 3 for light-colored products specified in the national standard, meeting the relevant standards and can enter the next round of testing.

[0069] Table 2

[0070]

[0071] From Table 2, we can see

[0072] Comparing the performance of the yarn after dyeing in Examples 1, 2, 3, and 4, we found that the yarns in Examples 1 and 2 showed almost no coloring effect, and their K / S values ​​were greatly different from those of the dyed apocynum yarn in Example 4. Although the yarn in Example 3 showed a certain color change after dyeing, after in-depth testing, its K / S value was improved compared with that in Examples 1 and 2, but it was still quite different from the K / S value of the yarn after dyeing in Example 4. Therefore, after comprehensive analysis of various data, it can be clearly seen that in the reactive orange X-GN dye solution, the biological salt has a positive promoting effect on the dyeing process of the apocynum yarn. In contrast, the single use of APTES did not show a significant promoting effect on the dyeing of the apocynum yarn. However, when APTES and the biological salt act synergistically, the biological salt can adjust the electrolyte concentration in the dye solution, thereby promoting the dyeing process. At the same time, due to its unique structure, during the dyeing process, the end containing the amino group of APTES is ionized into a cation in the dye solution and combined with the carboxyl group on the dye; while the other end containing the carboxyl group is tightly combined with the hydroxyl group on the fiber surface through a condensation reaction, thereby achieving a function similar to that of a fixing agent in traditional dyeing processes, thereby achieving a similar fixing effect to a certain extent.

[0073] Comparative Example 1

[0074] The process is basically the same as that in Example 1, except that in step S400, 1 g of biological salt is added to the dye solution at 25°C, stirred for 2-3 minutes, and then 5 mL of APTES is added and stirred for 2-3 minutes. After all the dye solution is added, it is stirred for another 20 minutes and placed in a 60°C environment for dyeing. The other steps are the same as those in Example 1.

[0075] Comparative Example 2

[0076] The method is basically the same as Example 1, except that in step S400, 1.5 g of biological salt is added to the dye solution at 25°C, stirred for 2-3 minutes, and then 5 mL of APTES is added and stirred for 2-3 minutes. After all the dye solution is added, it is stirred for another 20 minutes and placed in a 60°C environment for dyeing. The other steps are the same as Example 1.

[0077] Comparative Example 3

[0078] The method is basically the same as Example 1, except that in step S400, 2 g of biological salt is added to the dye solution at 25°C, stirred for 2-3 minutes, and then 5 mL of APTES is added and stirred for 2-3 minutes. After all the dye solution is added, it is stirred for another 20 minutes and placed in a 60°C environment for dyeing. The other steps are the same as Example 1.

[0079] Embodiment 4 The apocynum yarn of dyeing is as Figure 5As shown in the picture, it can be seen that the color of the dyed ramie yarn is relatively uniform, without obvious defects such as wrinkles, color spots and nodules. Figure 6-8 Corresponding to the dyed apocynum yarn in Examples 1-3, it can be seen from the figure that when the amount of biological salt is lower than 15 g / L, as the concentration of biological salt gradually increases, the color of the dyed apocynum yarn also deepens; when the amount of biological salt reaches 15 g / L, as the amount of biological salt increases, the chromaticity gradually decreases, and the dyeing effect becomes worse and worse.

[0080] The basic conditions and color fastness of the apocynum yarns of Comparative Examples 1-3 were tested and compared with Comparative Example 1. The test results are shown in Table 3.

[0081] The K / S values ​​and color fixation rates of the apocynum yarns of Comparative Examples 1-3 were tested and compared with the data of Comparative Example 1. The test results are shown in Table 4.

[0082] Table 3

[0083]

[0084]

[0085] When the amount of apocynum yarn is 2g, the amount of APTES is 50mL / L, the dyeing time is 4h, the weight of fabric is 0.5% (owf), the bath ratio is 1:50, and the dyeing temperature is 60°C, the color fastness grades of the dyed yarns with different amounts of biological salts are shown in Table 3. As can be seen from Table 3, under the conditions of different amounts of biological salts, the fastness grades of the dyed apocynum yarns can mostly reach above grade 4 except for the color fastness to soap washing. The wet friction fastness of comparative examples 1 and 2 is relatively low, only reaching the lowest grade 3 of the national standard. The soap washing fastness of the yarns dyed with different amounts of biological salts has been tested and all reached the lowest grade 3 of the national standard, which meets the national standards and can be tested in the next step.

[0086] Table 4

[0087]

[0088] As shown in Table 4, after dyeing, the apocynum yarn shows a uniform coloring effect, which is due to the dyeing method used to ensure that the dye is uniformly and effectively attached to the yarn. When compared with Example 4, we found that the K / S value between the sample of Comparative Example 2 and Example 4 is slightly different, and the maximum value of the K / S value of Comparative Example 2 is much greater than the maximum value of the K / S value of Example 4. Behind this phenomenon, it may be attributed to the fact that in the range of biological salt concentration below 15g / L, biological salt plays a positive role, which promotes the interaction between dye molecules and yarn by reducing the negative charge on the surface of apocynum yarn, thereby enhancing the dyeing effect. Therefore, in this concentration range, with the gradual increase of biological salt concentration, the dyeing effect also shows a corresponding enhancement trend. However, when the biological salt concentration exceeds 15g / L, the situation is reversed. Excessive electrolyte concentration leads to enhanced interaction between dye molecules in the solution, prompting them to aggregate and even form precipitation. This change hinders the effective combination of dye molecules with apocynum yarn, limiting the further adsorption and fixation of dyes on yarn. Therefore, in an environment where the concentration of biological salts is higher than 15 g / L, although the concentration of biological salts in the dye solution is increasing, the dyeing effect of the apocynum yarn is not significantly improved, and may even be weakened due to dye aggregation. In summary, the conditions set in Comparative Example 2, that is, the concentration of biological salts is within an appropriate range, provide an optimal environment for the dyeing of apocynum yarn, ensuring the uniformity of the dyeing effect and a high degree of consistency with the standard sample.

[0089] Comparative Example 4

[0090] The method is basically the same as Example 1, except that in step S400, 1.5 g of biological salt is added to the dye solution at 25°C, stirred for 2-3 minutes, and then 2.5 mL of APTES is added and stirred for 2-3 minutes. After all the dye solution is added, it is stirred for another 20 minutes and placed in an environment of 60°C for dyeing. The other steps are the same as Example 1.

[0091] Comparative Example 5

[0092] The method is basically the same as Example 1, except that in step S400, 1.5 g of biological salt is added to the dye solution at 25°C, stirred for 2-3 minutes, and then 7.5 mL of APTES is added and stirred for 2-3 minutes. After all the dye solution is added, it is stirred for another 20 minutes and placed in a 60°C environment for dyeing. The other steps are the same as Example 1.

[0093] Comparative Example 6

[0094] The process is basically the same as that in Example 1, except that in step S400, 1.5 g of biological salt is added to the dye solution at 25°C, stirred for 2-3 minutes, and then 10 mL of APTES is added and stirred for 2-3 minutes. After all the dye solution is added, it is stirred for another 20 minutes and placed in a 60°C environment for dyeing. The other steps are the same as those in Example 1.

[0095] Comparative Example 7

[0096] The method is basically the same as Example 1, except that in step S400, 1.5 g of biological salt is added to the dye solution at 25°C, stirred for 2-3 minutes, and then 12.5 mL of APTES is added and stirred for 2-3 minutes. After all the dye solution is added, it is stirred for another 20 minutes and placed in an environment of 60°C for dyeing. The other steps are the same as Example 1.

[0097] Comparative Example 2 The dyed apocynum yarn is as follows Figure 7 As shown, Figure 9-12 Corresponding to the dyed apocynum yarn in Example 4-7, it can be seen from the figure that as the amount of APTES increases gradually, the chromaticity of the dyed apocynum yarn becomes lighter, and the chromaticity is darkest when the amount of APTES is 2.5 mL.

[0098] The basic conditions and color fastness of the apocynum yarns of Comparative Examples 4-7 were tested and compared with Comparative Example 2. The test results are shown in Table 5.

[0099] The K / S values ​​and color fixation rates of the apocynum yarns of Comparative Examples 4-7 were tested and compared with the data of Comparative Example 2. The test results are shown in Table 6.

[0100] Table 5

[0101] Colour fastness to rubbing - dry Colour fastness to rubbing - wet Color fastness to light Color fastness to soap washing Color fastness to perspiration Comparative Example 2 3 4 5 3 5 Comparative Example 4 3-4 3 5 3 5 Comparative Example 5 4-5 3-4 5 4 5 Comparative Example 6 4-5 4 5 2-3 4 Comparative Example 7 4 4-5 5 2 4

[0102] When the amount of APTES in the yarn is 2g, the amount of biological salt is 15g / L, the dyeing time is 4h, the weight of the fabric is 0.5% (owf), the bath ratio is 1:50, and the dyeing temperature is 60℃, the color fastness grades of the yarns dyed with different amounts of APTES are shown in Table 5. As can be seen from Table 5, except for the soap fastness, the other color fastnesses do not show too much difference as a whole, basically maintaining above level 3, which meets the national standard, and the soap fastness is the lowest level of level 3 when the amount of APTES is less than 7.5mL, which meets the national minimum standard requirements, but when the amount of APTES is greater than 7.5mL, the pH value in the dye solution is too high due to the large amount of amino groups contained in APTES, which accelerates the hydrolysis process of the dye itself. This side effect directly leads to a decrease in the effective dyeing rate of the dye on the APTES yarn, affecting the final dyeing effect, causing the soap fastness of the dyed fabric to drop sharply to level 2, which cannot meet the minimum level requirements for soap fastness in the national standard.

[0103] Table 6

[0104]

[0105] It can be seen from Table 6 that after dyeing, the apocynum yarn exhibits good dyeing uniformity. A detailed comparison with Standard Sample 2 reveals that when the APTES dosage is set to 2.5 mL, the K / S value of the apocynum yarn in Comparative Example 4 is excellent. This performance can be attributed to the exquisite regulation of the APTES concentration under specific conditions. APTES, with its unique polyamino structure, has the effect of adjusting the pH value of the dye solution to alkaline at this concentration, which is related to its unique amphiphilic structure. This increase in pH significantly promotes the reaction of the dye with the cellulose component in the apocynum yarn. Specifically, the alkaline environment enhances the OH in the dye solution. - The concentration of these OH ions - Under appropriate conditions, ions can cause the swelling of apocynum fibers, providing more accessible surface area and adsorption space for dye molecules. At the same time, the unique amphiphilic structure of APTES also provides more binding sites for the binding between dye molecules and fibers, thereby effectively improving the dye uptake rate of apocynum yarn. However, it is worth noting that when the APTES concentration is too high, although it may be due to the OH in the solution at the beginning, - The further increase of ions accelerates the reaction rate of the dye and cellulose, but it also inevitably accelerates the hydrolysis process of the dye itself. This side effect directly leads to a decrease in the effective dyeing rate of the dye on the cellulose fiber, affecting the final dyeing effect. In summary, the condition setting in Comparative Example 4, that is, when the biological salt concentration is 15g / L and the APTES dosage is 2.5mL, achieves the best dyeing effect of the apocynum yarn, which not only ensures the uniformity of the dyeing, but also maximizes the utilization rate of the dye and the coloring ability of the fiber.

[0106] Comparative Example 8

[0107] The process is basically the same as that in Example 1, except that in step S400, 1.5 g of biological salt is added to the dye solution at 25°C, stirred for 2-3 minutes, and then 5 mL of APTES is added and stirred for 2-3 minutes. After all the dye solution is added, it is stirred for another 20 minutes, and the dyeing is carried out in a 60°C environment. In step S600, the color is oscillated at a constant temperature for 1 hour. The other steps are the same as those in Example 1.

[0108] Comparative Example 9

[0109] The process is basically the same as that in Example 1, except that in step S400, 1.5 g of biological salt is added to the dye solution at 25°C, stirred for 2-3 minutes, and then 5 mL of APTES is added and stirred for 2-3 minutes. After all the dye solution is added, it is stirred for another 20 minutes, placed in a 60°C environment for dyeing, and the color is oscillated at a constant temperature for 2 hours in step S600. The other steps are the same as those in Example 1.

[0110] Comparative Example 10

[0111] The process is basically the same as that in Example 1, except that in step S400, 1.5 g of biological salt is added to the dye solution at 25°C, stirred for 2-3 minutes, and then 5 mL of APTES is added and stirred for 2-3 minutes. After all the dye solution is added, it is stirred for another 20 minutes, placed in a 60°C environment for dyeing, and the color is oscillated at a constant temperature for 3 hours in step S600. The other steps are the same as those in Example 1.

[0112] Comparative Example 11

[0113] The process is basically the same as that in Example 1, except that in step S400, 1.5 g of biological salt is added to the dye solution at 25°C, stirred for 2-3 minutes, and then 5 mL of APTES is added and stirred for 2-3 minutes. After all the dye solution is added, it is stirred for another 20 minutes, and the dyeing is carried out in a 60°C environment. In step S600, the color is oscillated at a constant temperature for 5 hours. The other steps are the same as those in Example 1.

[0114] Comparative Example 4 The dyed apocynum yarn is as follows Fig. 9 As shown in the picture, it can be seen that the ramie yarn is dyed with uniform color, without defects such as wrinkles, color spots and nodules. Figure 12-16 Corresponding to the dyed apocynum yarn in Examples 8-11, it can be seen from the figure that with the change of dyeing time, the chromaticity of the dyed apocynum yarn also changes accordingly. When the dyeing time is less than 4 hours, the dyeing uniformity and depth gradually increase with the increase of dyeing time, but when the dyeing time is greater than 4 hours, the dyeing depth and uniformity tend to decrease.

[0115] The basic conditions and color fastness of the apocynum yarns of Comparative Examples 8-11 were tested and compared with the data of Comparative Example 4. The test results are shown in Table 7.

[0116] The K / S values ​​and color fixation rates of the apocynum yarns of Comparative Examples 8-11 were tested and compared with the data of Comparative Example 4. The test results are shown in Table 8.

[0117] Table 7

[0118] Colour fastness to rubbing - dry Colour fastness to rubbing - wet Color fastness to light Color fastness to soap washing Color fastness to perspiration Comparative Example 4 3-4 4 5 3 4-5 Comparative Example 8 4-5 3-4 5 2 4 Comparative Example 9 4-5 3 5 2-3 5 Comparative Example 10 4-5 3 5 2-3 5 Comparative Example 11 3-4 2 5 1-2 5

[0119] When the amount of apocynum yarn is 2g, the amount of biosalt is 15g / L, the amount of APTES is 25mL / L, the weight of fabric is 0.5% (owf), the bath ratio is 1:50, and the dyeing temperature is 60℃, the color fastness grades of the yarns after dyeing at different dyeing times are as follows: Figure 7 As shown. The overall dry rubbing fastness shows a downward trend with the increase of dyeing time, and the overall wet rubbing fastness is above level 3. The yarn with a dyeing time of 5h has a large dyeing difference in yarns in different regions due to the long dyeing time, which makes its color fastness level worse than the wet rubbing fastness of other samples. It can be seen from the above table that the perspiration fastness and light fastness of samples with different dyeing times have small differences. The light fastness is above level 5, and the perspiration fastness is above level 4. For samples with different dyeing times, as time increases, the soap washing fastness first increases and then decreases, reaching level 3 at 4h, which meets the minimum national dyeing standard requirements. The samples with other dyeing times are all below level 3.

[0120] Table 8

[0121]

[0122] From Table 8, we can see

[0123] Dyeing time has a significant impact on the dyeing effect. If the dyeing time is too long, the color of the material surface may become too dark, and even cause uneven flowery phenomenon, which is particularly prominent in light-colored dyeing. By comparing and analyzing Comparative Example 4 with Comparative Example 8, Comparative Example 9, and Comparative Example 10, we found that the dyeing time of these comparative examples is too short, resulting in the inability of the dye to fully penetrate into the interior of the material, so that the color is lighter and easy to fade. In particular, the dyeing effect of the apocynum yarn of Comparative Example 8 and Comparative Example 9 is extremely poor, the color is lighter and the leveling rate is low, and the established dyeing quality standards cannot be met. In contrast, the dyeing time of Comparative Example 11 is too long, resulting in a decrease in the leveling degree of the yarn, and the K / S value (i.e., the measurement of dyeing depth or concentration) in different regions is significantly different, and the dyeing requirements are also not met. Considering various factors, the dyeing result obtained by Comparative Example 4 under the set dyeing conditions is more ideal.

[0124] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as limiting the present invention.

[0125] In addition, the terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined as "first" and "second" may explicitly or implicitly include at least one of the features. In the description of the present invention, the meaning of "plurality" is at least two, such as two, three, etc., unless otherwise clearly and specifically defined.

[0126] In the present invention, unless otherwise clearly specified and limited, the terms "installed", "connected", "connected", "fixed" and the like should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements, unless otherwise clearly defined. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0127] In the present invention, unless otherwise clearly specified and limited, a first feature being "above" or "below" a second feature may mean that the first and second features are in direct contact, or the first and second features are in indirect contact through an intermediate medium. Moreover, a first feature being "above", "above" or "above" a second feature may mean that the first feature is directly above or obliquely above the second feature, or simply means that the first feature is higher in level than the second feature. A first feature being "below", "below" or "below" a second feature may mean that the first feature is directly below or obliquely below the second feature, or simply means that the first feature is lower in level than the second feature.

[0128] It should be noted that when an element is referred to as being "fixed to" or "disposed on" another element, it may be directly on the other element or there may be a central element. When an element is considered to be "connected to" another element, it may be directly connected to the other element or there may be a central element at the same time. The terms "vertical", "horizontal", "upper", "lower", "left", "right" and similar expressions used herein are for illustrative purposes only and are not intended to be the only implementation method.

Claims

1. A low-temperature one-bath dyeing method for apocynum yarn using biological salt from saline-alkali land, characterized in that: The following steps are included S100, at room temperature of 25°C, weigh saline-alkali soil and place it in an appropriate amount of distilled water, heat it in a water bath, filter it several times, and dry it to obtain saline-alkali soil biological salt for later use; S200, at room temperature of 25°C, completely immersing the impurity-removed apocynum yarn in distilled water at a temperature of 25°C, and wringing out excess water after the yarn is completely wet, so that the yarn is in a semi-dry state for standby use; S300, at room temperature 25°C, weigh an appropriate amount of reactive dye and place it in an appropriate amount of distilled water at a temperature of 25°C to prepare a dye solution with a concentration of 100 ppm for standby use; S400, placing the dye solution at a temperature of 25° C. in S300 into a constant temperature environment at 60° C.; S500, adding an appropriate amount of saline-alkali biological salt to the dye solution at a temperature of 25° C. to dissolve it; S600, adding an appropriate amount of silane coupling agent to the dye solution at a temperature of 25° C. to make it evenly dispersed; S700, when the temperature of the dye solution after fusion rises to 40°C, add the apocynum yarn to make it evenly dispersed; S800, when the temperature of the dye solution rises to 60℃, keep the dyeing at constant temperature for 4 hours, then wash and dry to achieve low-temperature dyeing of the apocynum yarn.

2. The low-temperature one-bath dyeing method for apocynum venetum yarn using saline-alkali land biological salt according to claim 1, characterized in that: The biological salt described in step S100 is biological salt extracted from saline-alkali land, and the concentration of the biological salt is 15 g / L.

3. The low-temperature one-bath dyeing method for apocynum venetum yarn using saline-alkali land biological salt according to claim 2, characterized in that: The process flow of the biological salt extraction is as follows: weigh an appropriate amount of saline-alkali soil and place it in an appropriate amount of distilled water at a temperature of 25°C, the mass ratio of saline-alkali soil to water is 1:20, heat it to 95°C in a water bath and stir it for 60 minutes, then let it stand and cool at room temperature, filter it three times after the solution is completely separated into upper and lower layers, take the supernatant, centrifuge it once, the speed is 10000 r / min, the processing time is 10 minutes, take the supernatant again and place it in a beaker, and treat it at 80°C for 24-48 hours.

4. The low-temperature one-bath dyeing method for apocynum venetum yarn using saline-alkali land biological salt according to claim 1, characterized in that: The amount of the apocynum yarn used in step S200 is 2 g.

5. The low-temperature one-bath dyeing method for apocynum venetum yarn using saline-alkali land biological salt according to claim 1, characterized in that: The amount of the reactive dye solution used in step S300 is 100 mL, the concentration of the reactive dye solution is 100 ppm, the dyeing dye is 0.5% by weight of the fabric, and the bath ratio is 1:

50.

6. The low-temperature one-bath dyeing method for apocynum venetum yarn using saline-alkali land biological salt according to claim 1, characterized in that: In step S500, 1.5 g of the saline-alkali land biological salt is added and stirred for 2-3 minutes.

7. The low-temperature one-bath dyeing method for apocynum venetum yarn using saline-alkali land biological salt according to claim 1, characterized in that: In step S600, 2.5 mL of the silane coupling agent is added and stirred for 2-3 min; the silane coupling agent is an aminosilane coupling agent, and the component of the aminosilane coupling agent is 3-aminopropyltriethoxysilane.

8. The low-temperature one-bath dyeing method for apocynum venetum yarn using saline-alkali land biological salt according to claim 1, characterized in that: In step S700, after all the saline-alkali land biological salt and the silane coupling agent are added to the dye solution, the solution is stirred for 20 minutes and the temperature is raised to 40°C.

9. The low-temperature one-bath dyeing method for apocynum venetum yarn using saline-alkali land biological salt according to claim 1, characterized in that: In step S800, the temperature of the apocynum yarn is raised to 60° C., and the temperature is kept constant for 60 minutes. The apocynum yarn is taken out, washed, and dried.

10. The low-temperature one-bath dyeing method for apocynum venetum yarn using saline-alkali land biological salt according to claim 1 or 5, characterized in that: The reactive dye described in step S300 is reactive orange, and the mass concentration is 0.1%.