Natural dye synergistic mordanting method for high-color-depth wool fabric

By employing a ternary synergistic mordant method involving sour papaya extract, rare earth salts, and madder dye, the problems of insufficient dyeing depth and poor color fastness of madder were solved, achieving high color depth and environmentally friendly wool fabric dyeing, simplifying the operation process and improving production efficiency.

CN122013559APending Publication Date: 2026-05-12JIANGYIN POLYTECHNIC COLLEGE
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
JIANGYIN POLYTECHNIC COLLEGE
Filing Date
2026-02-06
Publication Date
2026-05-12

AI Technical Summary

Technical Problem

In existing technologies, direct dyeing of wool fabrics with madder has problems such as insufficient dyeing depth and poor color fastness. In addition, traditional mordant dyeing processes are cumbersome and have low production efficiency. The dyeing depth improvement of single or binary mordants is limited and cannot meet the industrial demand for high color depth.

Method used

A ternary synergistic mordant method using sour papaya extract, rare earth salts, and madder dye was adopted. By adding sour papaya extract and rare earth salts in a one-step bath, adjusting the pH value to 3-4, and raising the temperature to 95℃ for dyeing, the operation process was simplified and the dyeing depth and color fastness were improved.

Benefits of technology

It achieves high color depth and excellent color fastness dyeing of wool fabrics, simplifies the operation process, improves production efficiency, reduces mechanical and chemical damage to fibers, and has environmental protection properties.

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Abstract

The invention discloses a high-color-depth wool fabric natural dye synergistic mordanting method which comprises the following steps: cleaning a wool fabric, removing surface impurities, and draining for later use; adding the sour papaya slices into water, heating until the sour papaya slices are boiled and then are slightly boiled, keeping the slightly boiling state, carrying out heat-preservation extraction, and filtering to obtain a sour papaya extracting solution; adding deionized water into a dyeing container according to a bath ratio, sequentially adding madder dye, a chaenomeles speciosa extracting solution and rare earth salt, and adjusting the pH value of a dye bath to 3-4; immersing the wool fabric into the dye liquor, raising the temperature to 95 DEG C, and keeping the temperature for dyeing; after the dyeing is finished, carrying out post-treatment to obtain the high-color-depth wool fabric. Through the synergistic complexing effect of the rare earth ions, polyphenol substances in the chaenomeles speciosa extracting solution and the rubia cordifolia dye, the dyeing depth and color fastness of the wool fabric are remarkably improved, and the problem that the direct dyeing depth of natural dye is insufficient is solved; the one-bath one-step method is simple in process, efficient and environment-friendly, and damage to the fibers is reduced.
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Description

Technical Field

[0001] This invention relates to the field of textile dyeing technology, specifically to a method for synergistic mordant dyeing of high-color, deep-dark wool fabrics with natural dyes. Background Technology

[0002] Wool fabrics, as natural protein fiber products, possess excellent wearing properties such as softness, warmth, and skin-friendliness, making them highly favored by consumers. Natural dyes, derived from plants, animals, or minerals in nature, have advantages such as being environmentally friendly, non-toxic, and biodegradable, aligning with the current trend of green textile development and showing broad application prospects in wool fabric dyeing.

[0003] Madder is a traditional natural red dye, with its active dyeing components being anthraquinone compounds that interact with wool fibers to achieve dyeing. However, when madder is used directly to dye wool, problems such as insufficient dyeing depth and poor color fastness exist, making it difficult to meet the needs of industrial production and practical use. To solve these problems, existing technologies mostly employ mordant dyeing processes. Common mordants include single mordants such as aluminum salts, iron salts, and rare earth salts, but the synergistic effect of single mordants is limited.

[0004] Sour papaya, as a natural plant material, contains polyphenolic tannins in its extract, which can act as a natural mordant synergist, working synergistically with mordants to improve dyeing effects. However, there are currently no reports on combining sour papaya extract, rare earth salts, and madder dye in a one-step, single-bath dyeing process for wool fabrics. Traditional pre-mordant or post-mordant processes suffer from drawbacks such as cumbersome operation, low production efficiency, and poor dyeing uniformity. Furthermore, the improvement in dyeing depth achieved by a single mordant or a binary mordant combination is limited, failing to meet the demand for high-depth dyeing.

[0005] Therefore, developing a natural dyeing process for wool fabrics that is simple, has high dyeing depth, excellent color fastness, and causes little damage to fibers has become an urgent technical problem to be solved in this field. Summary of the Invention

[0006] The purpose of this invention is to provide a method for synergistic mordating of high-color-density wool fabrics with natural dyes, so as to solve the problems mentioned in the background art.

[0007] To achieve the above objectives, the present invention provides the following technical solution: a method for synergistic mordating of high-color-depth wool fabrics with natural dyes, comprising the following steps: S1: After washing the wool fabric to remove surface impurities, drain it and set it aside. S2: Add sour papaya slices to water, heat to boiling and then reduce to a gentle boil, maintain this gentle boil state for a period of time for extraction, and filter to obtain sour papaya extract. S3: Add madder dye, deionized water, acid papaya extract prepared in step S2 and rare earth salt to the dyeing container in sequence according to the bath ratio, and adjust the pH value of the dye bath to 3-4. S4: Immerse the wool fabric treated in step S1 into the dyeing solution of step S3, raise the temperature to 95°C and keep it warm for dyeing. S5: After dyeing, the wool fabric is rinsed and soaped, and then dried to obtain a high-color, dark wool fabric.

[0008] Preferably, in step S3, the rare earth salt is lanthanum chloride.

[0009] Preferably, the amount of rare earth salt used is 3% to 5% of the weight of the wool fabric.

[0010] Preferably, the amount of rare earth salt used is 5% of the weight of the wool fabric.

[0011] Preferably, in step S3, the pH value of the dye bath is 3.

[0012] Preferably, in step S2, the ratio of the sour papaya slices to water is 50g:500mL, and the heat preservation time in the simmering state is 30min.

[0013] Preferably, in step S3, the liquor ratio is 1:30, the amount of madder dye used is 2% owf of the wool fabric mass, and the amount of acid papaya extract used is calculated based on 0.5 mL / 1 g wool mass.

[0014] Preferably, in step S4, the heating rate is 1℃ / min, the holding and staining time is 60min, and stirring is performed during the staining process.

[0015] Preferably, step S1 includes immersing the wool fabric in deionized water and washing it at 80°C for 30 minutes to remove surface impurities and drain it.

[0016] Preferably, the soaping treatment uses a 2g / L neutral soap flake detergent solution, and is treated at 80°C for 15 minutes.

[0017] This invention utilizes the synergistic effect of rare earth salts, sour papaya extract, and madder dye to enhance the dyeing depth and color fastness of wool fabrics by leveraging the strong complexing and synergistic effect of polyphenolic tannins in sour papaya and rare earth ions.

[0018] At the same time, the ternary complex system enhances the binding force between dye molecules and fibers, effectively improving the shortcomings of insufficient fastness in traditional dyeing processes.

[0019] In addition, the one-step method in the same bath simplifies the operation process and improves production efficiency. It also optimizes the amount of chemicals used through synergistic mordant dyeing, reducing mechanical and chemical damage to wool fibers. It has excellent environmental performance and promising prospects for industrial application. Attached Figure Description

[0020] Figure 1 These are comparative photographs of the dyed wool fabrics obtained in Example 1 of the present invention and Comparative Examples 1-3. Figure 2 These are comparative photographs of dyed wool fabrics obtained with different amounts of rare earth salts according to the present invention. Figure 3 These are comparative photographs of dyed wool fabrics obtained by using different amounts of acid papaya extract according to the present invention. Detailed Implementation

[0021] This invention provides a method for synergistic mordating of high-color, deep-dark wool fabrics with natural dyes, comprising the following steps: S1: After washing the wool fabric to remove surface impurities, drain it and set it aside. S2: Add sour papaya slices to water, heat to boiling and then reduce to a gentle boil, maintain this gentle boil state for a period of time for extraction, and filter to obtain sour papaya extract. S3: Add madder dye, deionized water, acid papaya extract prepared in step S2 and rare earth salt to the dyeing container in sequence according to the bath ratio, and adjust the pH value of the dye bath to 3-4. S4: Immerse the wool fabric treated in step S1 into the dyeing solution of step S3, raise the temperature to 95°C and keep it warm for dyeing. S5: After dyeing, the wool fabric is rinsed and soaped, and then dried to obtain a high-color, dark wool fabric.

[0022] In step S3, the rare earth salt is lanthanum chloride, and the amount of rare earth salt used is 3% to 5% of the weight of the wool fabric.

[0023] The preferred amount of rare earth salt is 5% of the weight of the wool fabric.

[0024] In step S3, the pH value of the dye bath is 3.

[0025] In step S2, the ratio of sour papaya slices to water is 50g:500mL, and the heat preservation time under simmering conditions is 30min.

[0026] In step S3, the liquor ratio is 1:30, the amount of madder dye used is 2% owf of the wool fabric mass, and the amount of sour papaya extract is added based on 0.5 mL / 1g wool mass.

[0027] In step S4, the heating rate is 1℃ / min, the staining time is 60min, and stirring is performed during the staining process.

[0028] Step S1 includes immersing the wool fabric in deionized water and washing it at 80°C for 30 minutes to remove surface impurities and drain it.

[0029] The soaping treatment used a 2g / L neutral soap flake detergent solution, and was treated at 80℃ for 15 minutes.

[0030] Example 1 Take 2g of wool fabric, immerse it in deionized water, and wash it at 80℃ for 30 minutes to remove grease, dust and other impurities from the surface of the fabric. After washing, take out the wool fabric, let it drain naturally and set it aside.

[0031] Weigh 50g of sour papaya slices, add 500mL of distilled water, boil on an induction cooker and keep warm for 30 minutes, filter and make up to 500mL to obtain sour papaya extract, refrigerate for later use.

[0032] Add 10 ml of madder stock solution (2% owf, madder stock solution concentration is 4 g / L) to the staining cup, add 49 mL of deionized water (bath ratio 1:30), 1.0 mL of acid papaya extract, adjust the pH of the staining bath to 3 with glacial acetic acid solution, and then add 0.1 g of lanthanum chloride (5% owf).

[0033] The pretreated wool fabric is immersed in the dye bath and heated to 95°C at a rate of 1°C / min, and kept at that temperature for 60 minutes, during which time it is stirred.

[0034] After dyeing, remove the wool fabric, rinse with cold water, wash with 2g / L neutral soap flake detergent at 80℃ for 15min, rinse with cold water, and air dry to obtain a high-color, deep-dark wool fabric.

[0035] To verify the technical effectiveness of the present invention, the following comparative examples were used for performance testing: Comparative Example 1: Madder dyeing process without adding sour papaya extract and rare earth salts Take 2g of wool fabric and pretreat it in the same way as in Example 1, that is: immerse the wool fabric in deionized water, wash it at 80°C for 30 minutes, remove surface impurities, and drain it naturally for later use.

[0036] The dye bath was prepared as follows: 10 mL of madder mother liquor (2% owf, madder mother liquor concentration of 4 g / L) was added to the dye cup, and then deionized water was added to keep the total volume of the dye bath consistent with that in Example 1, with a bath ratio of 1:30; no acid papaya extract or lanthanum chloride was added, and the pH of the dye bath was adjusted to 3 with glacial acetic acid solution.

[0037] The pretreated wool fabric was immersed in the dye solution. Under the same stirring conditions as in Example 1, the temperature was increased to 95°C at a rate of 1°C / min and held at that temperature for 60 minutes to complete the dyeing process.

[0038] After dyeing, the wool fabric was removed and then rinsed with cold water, washed with 2g / L neutral soap flakes at 80℃ for 15 minutes, rinsed with cold water and dried to obtain the dyed wool fabric.

[0039] Comparative Example 2: Madder dyeing process with the addition of sour papaya extract but without the addition of rare earth salts Take 2g of wool fabric and pretreat it in the same way as in Example 1, that is: immerse the wool fabric in deionized water, wash it at 80°C for 30 minutes, remove surface impurities, and drain it naturally for later use.

[0040] The sour papaya extract was prepared according to the method described in Example 1 and stored under cold for later use.

[0041] The dye bath was prepared as follows: 10 mL of madder mother liquor (2% owf, madder mother liquor concentration is 4 g / L) was added to the dye cup, followed by 1.0 mL of acid papaya extract and deionized water, so that the total volume of the dye bath was consistent with that in Example 1, and the bath ratio was 1:30; lanthanum chloride was not added, and the pH of the dye bath was adjusted to 3 with glacial acetic acid solution.

[0042] The pretreated wool fabric was immersed in the dye solution. Under the same stirring conditions as in Example 1, the temperature was increased to 95°C at a rate of 1°C / min and held at that temperature for 60 minutes to complete the dyeing process.

[0043] After dyeing, the wool fabric was removed and then rinsed with cold water, washed with 2g / L neutral soap flakes at 80℃ for 15 minutes, rinsed with cold water and dried to obtain the dyed wool fabric.

[0044] Comparative Example 3: Madder dyeing process with the addition of rare earth salts but without the addition of acidic papaya extract Take 2g of wool fabric and pretreat it in the same way as in Example 1, that is: immerse the wool fabric in deionized water, wash it at 80°C for 30 minutes, remove surface impurities, and drain it naturally for later use.

[0045] The dye solution was prepared as follows: 10 mL of madder stock solution (2% owf, madder stock solution concentration of 4 g / L) was added to the dye cup, and then deionized water was added to make the total volume of the dye bath consistent with that in Example 1, with a bath ratio of 1:30; no acid papaya extract was added, and the pH of the dye bath was adjusted to 3 with glacial acetic acid solution, and then 0.1 g of lanthanum chloride (5% owf) was added.

[0046] The pretreated wool fabric was immersed in the dye solution. Under the same stirring conditions as in Example 1, the temperature was increased to 95°C at a rate of 1°C / min and held at that temperature for 60 minutes to complete the dyeing process.

[0047] After dyeing, the wool fabric was removed and then rinsed with cold water, washed with 2g / L neutral soap flakes at 80℃ for 15 minutes, rinsed with cold water and dried to obtain the dyed wool fabric.

[0048] Performance testing: The dyed wool fabrics obtained in Example 1 and Comparative Examples 1-3 were subjected to performance tests. Dyeing performance was characterized using a computer-aided colorimeter, and the K / S value and L, a, and b characteristic parameters of the fabrics were measured. Different parts of each fabric were measured four times, and the average value was taken as the test result. The test results are shown in the table below.

[0049] First, comparing Comparative Example 1 and Comparative Example 2, it can be seen that when only the sour papaya extract is introduced into the madder dyeing system (Comparative Example 2), the K / S value of the wool fabric is higher than that of Comparative Example 1, which is directly dyed with madder, but the increase is limited. At the same time, the corresponding L value is still at a high level, indicating that the polyphenolic components contained in the sour papaya extract can play an auxiliary role in the dyeing process to a certain extent, but its effect on improving the dyeing depth is still relatively limited when no metal mordant components are introduced.

[0050] Secondly, comparing Comparative Example 1 and Comparative Example 3, it can be seen that after introducing rare earth salts as mordants into the madder dyeing system (Comparative Example 3), the K / S value of the resulting wool fabric is significantly higher than that of Comparative Example 1 and Comparative Example 2, and the L value is significantly reduced. This indicates that rare earth ions, as mordant components, are beneficial to enhancing the fixation ability of madder dye on wool fibers, thereby improving the dyeing depth. However, under the condition of a binary system consisting only of rare earth salts and dyes, there is still room for further improvement in its dyeing effect.

[0051] Further comprehensive comparison of Example 1 and the comparative examples reveals that, under the condition of simultaneously introducing sour papaya extract and rare earth salt, the K / S value of the wool fabric obtained in Example 1 is further improved, and the corresponding L value is the lowest, with the fabric color being the deepest. This indicates that in the dyeing system of the present invention, the synergistic introduction of sour papaya extract and rare earth salt is beneficial to further improve the dyeing effect of madder dye, and its overall color performance is significantly better than that of the dyeing system that only introduces a single component, demonstrating a significant synergistic effect.

[0052] Based on the above experimental results, in order to further leverage the advantages of this synergistic staining system and determine the appropriate dosage range of each functional component, this invention further systematically optimized the effects of rare earth salt dosage and sour papaya extract dosage on staining performance. Furthermore, the effect of rare earth salt (lanthanum chloride) dosage on staining performance was investigated.

[0053] The following experiments were all conducted under the same dyeing process and testing methods as in Example 1, with only the amount of rare earth salt (lanthanum chloride) being changed. The results are mainly used to reflect the trend of the effect of the change in the amount of rare earth salt on the dyeing performance. The specific values ​​between different test batches may have some differences.

[0054] Specifically, the rare earth salt dosages were set to 1%, 2%, 3%, 5%, and 8% (by fabric weight, owf), respectively. The K / S value and L, a, and b parameters of the wool fabrics obtained under different dosage conditions were tested, and the results are shown in the table below: The test results show that the K / S value of the fabric generally increases with the increase of rare earth salt dosage, with a particularly significant increase in the range of 3% to 5% owf. When the rare earth salt dosage is 5% owf, the fabric achieves a higher K / S value and a lower L value, resulting in a more ideal dyeing effect. Further increasing the rare earth salt dosage to 8% owf leads to a gradual decrease in K / S. Considering both dyeing effect and process feasibility, a rare earth salt dosage range of 3% to 5% owf is considered suitable, with 3% owf being one of the preferred conditions for balancing dyeing effect and dosage control.

[0055] The effect of the amount of sour papaya extract on staining performance was further investigated.

[0056] The following experiments were conducted under the same dyeing process and testing methods as in Example 1, with only the amount of sour papaya extract being changed. The results are mainly used to reflect the trend of the effect of changes in the amount of sour papaya extract on the dyeing performance. The specific values ​​between different test batches may vary to some extent.

[0057] Specifically, the amounts of sour papaya extract used were set to 0.25 mL, 0.5 mL, 1.0 mL, 3.0 mL, and 5.0 mL (corresponding to 2 g of wool fabric), respectively. The K / S value and L, a, and b parameters of the resulting fabrics were tested, and the results are shown in the table below: The results showed that the K / S value of the fabric first increased and then decreased with the increase of the amount of papaya extract. When the amount of papaya extract was 1.0 mL, the fabric obtained a higher K / S value and a lower L value, and the dyeing effect was more ideal. When the amount was further increased, the K / S value decreased significantly, indicating that excessive addition was not conducive to further improvement of the dyeing depth. Therefore, under the process conditions of this invention, the amount of papaya extract is more suitable in the range of 0.5 to 1.0 mL, with 1.0 mL being the preferred condition.

[0058] In summary, this invention, by synergistically introducing acidic papaya extract and rare earth salts into the madder dyeing system, and under the condition of reasonable control of the dosage of each component, can significantly improve the dyeing depth and enhance the color characteristic parameters of wool fabrics. This method effectively improves the dyeing effect of natural dyes while maintaining the stability and feasibility of the dyeing process, and has promising application prospects.

[0059] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely preferred examples and are not intended to limit the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the present invention as claimed. The scope of protection of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for synergistic mordating of high-color, deep-dark wool fabrics with natural dyes, characterized in that: Includes the following steps S1: After washing the wool fabric to remove surface impurities, drain and set aside. S2: Add sour papaya slices to water, heat to boiling and then reduce to a gentle boil, maintain this gentle boil state for a period of time for extraction, and filter to obtain sour papaya extract. S3: Add madder dye, deionized water, acid papaya extract prepared in step S2 and rare earth salt to the dyeing container in sequence according to the bath ratio, and adjust the pH value of the dye bath to 3-4. S4: Immerse the wool fabric treated in step S1 into the dyeing solution of step S3, raise the temperature to 95°C and keep it warm for dyeing. S5: After dyeing, the wool fabric is rinsed and soaped, and then dried to obtain a high-color, dark wool fabric.

2. The method for synergistic mordating of high-color, deep-dark wool fabrics with natural dyes according to claim 1, characterized in that: In step S3, the rare earth salt is lanthanum chloride.

3. The method for synergistic mordating of high-color, deep-dark wool fabrics with natural dyes according to claim 2, characterized in that: The amount of rare earth salt used is 3% to 5% of the weight of the wool fabric.

4. The method for synergistic mordating of high-color, deep-dark wool fabrics with natural dyes according to claim 3, characterized in that: The amount of rare earth salt used is 5% of the weight of the wool fabric.

5. The method for synergistic mordating of high-color, deep-dark wool fabrics with natural dyes according to claim 1, characterized in that: In step S3, the pH value of the dye bath is 3.

6. The method for synergistic mordating of high-color, deep-dark wool fabrics with natural dyes according to claim 1, characterized in that: In step S2, the ratio of the sour papaya slices to water is 50g:500mL, and the heat preservation time under the simmering state is 30min.

7. The method for synergistic mordating of high-color, deep-dark wool fabrics with natural dyes according to claim 1, characterized in that: In step S3, the liquor ratio is 1:30, the amount of madder dye used is 2% owf of the wool fabric mass, and the amount of acid papaya extract used is calculated based on 0.5 mL / 1 g wool mass.

8. The method for synergistic mordating of high-color, deep-dark wool fabrics with natural dyes according to claim 1, characterized in that: In step S4, the heating rate is 1℃ / min, the holding time for staining is 60min, and stirring is performed during the staining process.

9. The method for synergistic mordating of high-color, deep-dark wool fabrics with natural dyes according to claim 1, characterized in that: Step S1 includes immersing the wool fabric in deionized water and washing it at 80°C for 30 minutes to remove surface impurities and drain it.

10. The method for synergistic mordating of high-color, deep-dark wool fabrics with natural dyes according to claim 1, characterized in that: The soaping treatment uses a 2g / L neutral soap flake detergent solution, and is treated at 80℃ for 15 minutes.