Treatment methods for irreversible discoloration of cellulose fiber products after dyeing

By dyeing cellulose fiber products with dual-active or multi-active-group reactive dyes followed by amination treatment, the problems of rough hand feel and poor washability of color-changing fabrics are solved, achieving high color fixation rate and irreversible color change, and possessing good antibacterial properties and a soft hand feel.

CN116949844BActive Publication Date: 2026-03-10LUTAI TEXTILE
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-08-15
Publication Date
2026-03-10

AI Technical Summary

Technical Problem

Existing color-changing fabrics have a rough feel, poor washability, low dye fixation rate, complex production process, and limited selectivity, making it impossible to achieve irreversible color change in cellulose fiber products.

Method used

After dyeing with dual-reactive-group or multi-reactive-group reactive dyes, the cellulose fiber products are amination treated by covalent bonding reaction between amine compounds and unreacted reactive groups under specific conditions, achieving irreversible color change, and the process is carried out in a package dyeing machine or an overflow dyeing machine.

Benefits of technology

It improves the color fixation rate of cellulose fiber products to 70%-85%, imparts good antibacterial properties, has a soft hand feel, long-lasting washability, and is simple to operate and industrially feasible.

✦ Generated by Eureka AI based on patent content.

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Patent Text Reader

Abstract

This invention belongs to the field of textile technology, specifically relating to a method for treating irreversible discoloration of dyed cellulose fiber products. The method for treating irreversible discoloration of dyed cellulose fiber products according to this invention includes the following steps: (1) pretreatment of the cellulose fiber products; (2) dyeing of the cellulose fiber products, wherein sodium sulfate and soda ash are added during the dyeing process, and post-treatment is performed after dyeing; (3) amination treatment, wherein amine compounds and fatty alcohol polyoxyethylene ether emulsifier are added to the dyeing machine, and the mixture is heated. This invention has a simple process, is easy to operate, and has strong industrial feasibility; in addition to achieving irreversible discoloration of the dyed yarn, it also imparts good antibacterial properties to the fiber products. Compared with traditional coating finishing discoloration, the amination treatment method has the characteristics of soft hand feel and long-lasting washability.
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Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of textiles, and particularly relates to a treatment method for irreversible color change of dyed cellulose fiber products. BACKGROUND

[0002] With the improvement of the quality of life, more and more people pursue the diversity of clothes, and clothes are no longer just functional products for keeping warm, but also a display of personal taste. Nowadays, young people like to be different and pursue individuality. Color-changing fabrics are increasingly favored by young people.

[0003] There are many patents or documents about the finishing and processing method of color-changing fabrics, but most of the color-changing fabrics are finished by coating, which has rough and hard hand feeling, poor washing resistance, and cannot guarantee the persistent color-changing effect. The purpose of the present application is to overcome the shortcomings of the current color-changing fabrics, and provide a method for amine treatment of color change of cellulose fiber yarn or fabric.

[0004] In the document "Synthesis and application of high molecular active dye based on polyethylene imine structure", it is mentioned that a high molecular polymer is grafted on the dye matrix, and then the dye is dyed on the yarn or fabric by adding no sodium sulphate or soda ash or adding sodium sulphate or soda ash, which has a low dye fixation rate and greatly limits the practical application of the dye.

[0005] Patent CN104249534A discloses a processing method of cotton fabric super-hydrophobic coating color-changing fabric, and the surface of the fabric body is coated with a color-changing coating, which is a heat-sensitive compound. The coating color-changing fabric has the characteristics of rough and hard hand feeling and poor washing resistance.

[0006] Patent CN103556491A discloses a color point color-changing yarn or fabric and a processing method thereof. In this patent, cotton yarn or fabric is subjected to cationic modification treatment, and then special segment dyeing or spray dyeing is performed by using a heat-sensitive color-changing dye with a micro-gel structure to obtain a special style of color-changing yarn or fabric. The cationic modification treatment temperature is 60-80℃, and the time is 20-40 minutes. The production process is relatively complex, and the selection of dyes is limited.

[0007] The method of the present application provides a processing method for irreversible color change treatment of dyed cellulose fiber products, and provides customers and consumers with the choice of diversity. The method of amine color change treatment of cellulose fiber or fabric in the present application has not been reported in any patent or document. SUMMARY

[0008] In view of the deficiencies of the prior art, the present application aims to provide a method for treating irreversible color change of dyed cellulose fiber products, which uses commonly used double active group or multi active group reactive dyes, and has a high fixation rate of 70-85%, and has great application value.

[0009] The method for treating irreversible color change of dyed cellulose fiber products comprises the following steps:

[0010] (1) Pretreatment of cellulose fiber products

[0011] The cellulose fiber products are pretreated using a pretreatment agent; impurities, grease and the like are removed to improve the capillary effect of the cellulose fiber products.

[0012] (2) Dyeing of cellulose fiber products

[0013] Sodium sulfate and soda ash are added during the dyeing process, and post-treatment is performed after dyeing.

[0014] (3) Amination treatment

[0015] Different equipment is used for amination treatment of the cellulose fiber products according to the type of the cellulose fiber products, an amine compound and a fatty alcohol polyoxyethylene ether emulsifier are added to the equipment, the temperature is raised, and then the water is drained, and then the cellulose fiber yarn or fabric after amination treatment is washed with hot water.

[0016] The cellulose fiber product is one or more than two kinds of cotton fiber, Tencel fiber, flax fiber, viscose fiber, bamboo fiber blended yarn or fabric, the fineness of the yarn is 6-60 tex, the mass of the cheese is 0.3-1.0 kg, and the grammage of the fabric is 100-280 g / m 2 .

[0017] The mass ratio of the cellulose fiber product to water during the pretreatment, dyeing treatment, post-treatment and amination treatment is 1:(6-20).

[0018] The pretreatment of the cellulose fiber product in step (1) uses a pretreatment agent, which is a fatty alcohol polyoxyethylene ether emulsifier, and more preferably WAM produced by Lurui Fine Chemical Co., Ltd., is used in an amount of 0.5-1.5 g / L, a refining agent, which is more preferably SA-E produced by Lurui Fine Chemical Co., Ltd., is used in an amount of 1-2 g / L, and oil-removing agent is used in an amount of 0.5-2 g / L, the treatment temperature is 85-100 DEG C, and the time is 10-20 min.

[0019] The dye used in the dyeing treatment in step (2) is a double active group or multi active group reactive dye.

[0020] The process conditions of the dyeing of the cellulose fiber product in step (2) are that the dyeing temperature is 50-90℃, the dyeing time is 40-60min, the amount of sodium sulfate is 10-80g / L, and the amount of soda ash is 4-25g / L.

[0021] The process conditions of the post-dyeing treatment in step (2) are that the soaping agent, preferably WO produced by Luwei Fine Chemical Co., Ltd., is used in an amount of 2-8g / L, the soaping temperature is 80-100℃, and the soaping time is 10-20min, and then hot water washing is performed, and the hot water washing temperature and time are the same as the soaping temperature and time.

[0022] The amine compound in step (3) is one of a high-molecular amine compound or an alkyl amine preparation or a mixture of both. The preferred auxiliary agent is FR (high-molecular amine compound) or auxiliary agent AIX (alkyl amine preparation), both of which are produced by Zibo Luwei Fine Chemical Co., Ltd.

[0023] The process of the amine treatment of the cellulose fiber product in step (3) is that the amine compound is used in an amount of 2-30g / L, the fatty alcohol polyoxyethylene ether emulsifier WAM (produced by Zibo Luwei Fine Chemical Co., Ltd.) is used in an amount of 0.5-1.5g / L, the treatment temperature is 70-120℃, and the time is 15-60min, and after the amine treatment, hot water washing is performed, and the hot water washing temperature is 80-100℃ and the time is 10-20min.

[0024] The amine treatment in step (3) is performed in a package dyeing machine for yarns, and in an overflow dyeing machine or a tenter for fabrics, and when the treatment is performed, the pump speed of the package dyeing machine is set to be between 80-98%, the flow direction is from inside to outside, the cloth speed of the overflow dyeing machine is 200-260m / min, the nip ratio of the tenter is 65-80%, the pre-drying temperature of the tenter is 80-120℃, the time is 1-3min, the temperature of the steaming machine is 100-120℃, and the steaming time is 15-30min.

[0025] In the technical solution of the present application, the hot water washing is performed at a temperature of 80-100℃ for 10-20min.

[0026] The method of the present application provides a processing method for performing irreversible color change treatment on a dyed cellulose fiber product, and provides customers and consumers with a variety of choices, and there is no patent or literature reported on the method of performing amine color change treatment on cellulose fibers or fabrics by using the method of the present application.

[0027] The main technical principle of the present application is that: after the cellulose fiber product dyed by the double active group or multi-active group reactive dye, there is still part of the active group not participating in the covalent reaction, on this basis, the amine compound is used for amine treatment of the dyed cellulose fiber product under specific reaction conditions, the amine modification agent, i.e. the amine compound, can further covalently bond with the unreacted active group under the condition and then be grafted onto the fiber. Since the amine compound grafted onto the dye will produce steric hindrance effect on the conjugated structure of the dye chromophore parent body, the maximum absorption wavelength of the dye will change, and then the color of the dyed fiber product will change.

[0028] Compared with the prior art, the present application has the following beneficial effects:

[0029] (1) The amine treatment of the cellulose fiber product in the present application is carried out in a cheese dyeing machine or an overflow dyeing machine, which is simple in process, easy to operate and strong in industrialization realization.

[0030] (2) The method described in the present application not only realizes the irreversible color change of the dyed yarn, but also gives the fiber product good antibacterial performance.

[0031] (3) The amine treatment color change method described in the present application has the characteristics of soft hand feeling and durable washability compared with the traditional coating finishing color change. BRIEF DESCRIPTION OF DRAWINGS

[0032] Figure 1 K / S value curve diagram of Example 1 and Comparative Example 1 of the present application;

[0033] Figure 2 K / S value curve diagram of Example 2 and Comparative Example 2 of the present application;

[0034] Figure 3 K / S value curve diagram of Example 3 and Comparative Example 3 of the present application;

[0035] Figure 4 K / S value curve diagram of Example 4 and Comparative Example 4 of the present application. DETAILED DESCRIPTION

[0036] The present application will be further described below in combination with examples, but the protection scope of the present application is not limited thereto.

[0037] All raw materials used in the examples are commercially available, except for special instructions.

[0038] Deoiling agent TF-101N is purchased from Zhejiang Chuanhua Chemical Co., Ltd.

[0039] Smoothing agent LUA is purchased from Zibo Luru Fine Chemical Co., Ltd.

[0040] Neutralizing acid PH-N is purchased from Zibo Luru Fine Chemical Co., Ltd.

[0041] Example 1

[0042] The yarn count of the pure cotton knitted fabric is 18.2 tex, the weave is single jersey, and the grammage is 140 g / m 2 , and the specific treatment process is as follows:

[0043] (1) The pure cotton knitted fabric is pretreated, the dosage of emulsifier WAM is 1 g / L, the dosage of refining agent SA-E is 1 g / L, the dosage of deoiling agent TF-101N is 1 g / L, the rotating wheel speed of the dyeing machine is 230 m / min, the bath ratio is 1:10, the pretreatment temperature is 90℃, the time is 20 min, and after the pretreatment is completed, the pure cotton knitted fabric is washed once with hot water, the hot water washing temperature is 90℃, and the hot water washing time is 15 min;

[0044] (2) The pure cotton knitted fabric is dyed in an overflow dyeing machine, the dosage of dye ADBLUE is 1.0%, the dosage of sodium sulfate is 30 g / L, the dosage of sodium carbonate is 15 g / L, the mass ratio of the fabric to water is 1:10, the rotating wheel speed of the dyeing machine is 240 m / min, the temperature rising rate is 1℃ / min, the dyeing temperature is 60℃, and the holding time is 60 min. After the dyeing is completed, soaping, hot water washing, and cold water washing are sequentially performed, the dosage of soaping agent WO is 5 g / L, the soaping temperature is 90℃, the soaping time is 15 min, the hot water washing temperature is 90℃, and the hot water washing time is 15 min;

[0045] (3) Amine treatment, the dosage of auxiliary FR is 20 g / L, the dosage of emulsifier WAM is 1 g / L, the fabric is dried by a tenter (the rolling rate of the rolling machine is 70%), the fabric is pre-dried at 90℃ for 1 min by a tenter, then the fabric is steamed at 110℃ for 20 min, and after the amine treatment is completed, the pure cotton fabric is washed once with hot water (the temperature is 90℃, and the hot water washing time is 15 min) and once with cold water (the cold water washing time is 15 min).

[0046] Example 2

[0047] The yarn count of the pure cotton knitted fabric is 14.58 tex, the weave is single jersey, and the grammage is 130 g / m 2 , and the specific treatment process is as follows:

[0048] (1) The pure cotton knitted fabric is pretreated, the dosage of emulsifier WAM is 1 g / L, the dosage of refining agent SA-E is 1 g / L, the dosage of deoiling agent TF-101N is 1 g / L, the rotating wheel speed of the dyeing machine is 220 m / min, the bath ratio is 1:10, the pretreatment temperature is 90℃, the time is 20 min, and after the pretreatment is completed, the pure cotton knitted fabric is washed once with hot water;

[0049] (2) Dyeing of the pure cotton knitted fabric in an overflow dyeing machine, dye BKSRFD: 2.0%, anhydrous sodium sulfate dosage 40 g / L, soda ash dosage 15 g / L, mass ratio of fabric to water 1:12, dyeing machine rotating wheel speed 240 m / min, temperature rising rate 1 °C / min, dyeing temperature 60 °C, holding time 60 min. After dyeing, carry out soaping, hot water washing in turn, soaping agent WO: 5 g / L, soaping temperature 90 °C, soaping time 15 min, hot water washing temperature 90 °C, hot water washing time 15 min,

[0050] (3) Amination treatment, auxiliary FR 1 g / L, AIX 8 g / L, emulsifier WAM dosage 1 g / L, amination treatment in an overflow dyeing machine, mass ratio of fabric to water 1:10, dyeing machine rotating wheel speed 240 m / min, amination treatment temperature 90 °C, treatment time 30 min. After amination treatment, carry out hot water washing (temperature 90 °C, hot water washing 15 min) and cold water washing (normal temperature water washing 15 min) each once on the pure cotton fabric.

[0051] Example 3

[0052] The fineness of the pure cotton cone yarn is 14.58 tex cotton fiber cone yarn, and the weight of the cone yarn is 0.9 kg. The specific processing process is as follows:

[0053] (1) Cotton fiber pretreatment, fatty alcohol polyoxyethylene ether emulsifier WAM dosage 1 g / L, refining agent SA-E dosage 1 g / L, oil removal agent TF-101N dosage 1 g / L, dyeing machine pump speed 90%, flow direction from inside to outside, bath ratio 1:8, pretreatment temperature 98 °C, time 15 min, after pretreatment, carry out hot water washing once on the pure cotton cone yarn, hot water washing temperature 90 °C, hot water washing time 15 min;

[0054] (2) Dyeing treatment of the pure cotton cone yarn, dye ADBLUE: 0.5% + AYELLOW: 0.5%, anhydrous sodium sulfate dosage 30 g / L, soda ash dosage 15 g / L, mass ratio of cone yarn to water 1:8, temperature rising rate 1 °C / min, dyeing temperature 60 °C, flow direction from inside to outside, holding time 60 min. After dyeing, carry out soaping, hot water washing in turn, soaping agent WO: 5 g / L, soaping temperature 95 °C, soaping time 10 min, hot water washing temperature 95 °C, hot water washing time 10 min.

[0055] (3) Amination treatment, amination auxiliary FR dosage 3 g / L, emulsifier WAM dosage 1 g / L, bath ratio 1:10, cone yarn dyeing machine pump speed setting 90%, flow direction from inside to outside, dyeing machine temperature 80 °C, treatment time 50 min, after amination treatment, carry out hot water washing (temperature 90 °C, hot water washing 15 min) and cold water washing (normal temperature water washing 15 min) each once on the pure cotton cone yarn.

[0056] (4) After the softening and drying after the amination treatment water washing, the softening treatment smoothing agent dosage 3.5% (percentage of the weight of the cheese), neutralizing acid PH-N: 0.9g / L, softening treatment temperature 55℃, softening treatment time 15min, cheese using radio frequency drying machine drying.

[0057] Example 4

[0058] In the example, Tencel yarn is selected, the fineness is 11.81tex, the weight of Tencel cheese is 0.5kg, and the specific processing process is as follows:

[0059] (1) Tencel yarn pretreatment, fatty alcohol polyoxyethylene ether emulsifier WAM dosage is 1g / L, oil removal agent dosage is 1g / L, refining agent SA-E dosage is 1g / L, dyeing machine pump speed is 90%, bath ratio is 1:9, pretreatment temperature is 98℃, time is 15min, after pretreatment, hot water washing is carried out once on Tencel cheese, hot water washing temperature is 90℃, hot water washing time is 15min;

[0060] (2) Tencel cheese is dyed, dye ADBLUE: 1.0%, sodium sulfate dosage 20g / L, soda ash dosage 4g / L, the mass ratio of cheese to water is 1:9, the heating rate is 1℃ / min, the dyeing temperature is 60℃, and the holding time is 60min. After dyeing, soaping, hot water washing are carried out in turn, soaping agent WO: 5g / L, soaping temperature is 90℃, soaping time is 10min, hot water washing temperature is 90℃, hot water washing time is 10min.

[0061] (3) Amination treatment, amination auxiliary agent FR 1g / L and AIX 15g / L, emulsifier WAM dosage is 1g / L, bath ratio 1:8, cheese dyeing machine pump speed is set to 90%, flow direction is from inside to outside, dyeing machine temperature is 80℃, treatment time is 40min, after amination treatment, hot water washing (temperature 90℃, hot water washing 15min) and cold water washing (normal temperature water washing 15min) are carried out once on Tencel cheese.

[0062] (4) After the softening and drying after the amination treatment water washing, the softening treatment smoothing agent dosage 3.5% (percentage of the weight of the cheese), neutralizing acid PH-N: 0.9g / L, softening treatment temperature 55℃, softening treatment time 15min, cheese using radio frequency drying machine drying.

[0063] Comparative examples 1-4:

[0064] Comparative Examples 1-4 are the same as the other steps of the amine treatment step in Examples 1-4. The color fixation rate, yarn K / S value, maximum absorption wavelength, antibacterial performance, and fastness of the yarn before and after treatment of Examples 1-4 and Comparative Examples 1-4 are tested, and the test results are shown in Table 1, and the fastness test results are shown in Table 2. The antibacterial performance test uses GB / T20944.3-2008 shock method, and the detected bacterial group is Staphylococcus aureus.

[0065] Table 1 Yarn performance after amine treatment

[0066]

[0067] Table 2 Yarn fastness after amine treatment

[0068] Examples and Comparative Examples Soaping fastness / grade Dry crocking fastness / grade Wet crocking fastness / grade Sunlight fastness / grade Example 1 4 / 5 4 / 5 3 / 4 3 Comparative Example 1 4 4 3 / 4 3 / 4 Example 2 4 4 / 5 3 3 Comparative Example 2 3 / 4 4 3 3 Example 3 4 4 / 5 3 / 4 3 Comparative Example 3 3 / 4 4 3 / 4 3 Example 4 4 4 3 / 4 3 Comparative Example 4 3 / 4 4 3 / 4 3

[0069] From the data in Table 1, the fabric / yarn prepared by the steps of Examples 1-4 of the present application has a changed K / S value, a significantly shifted maximum absorption wavelength, a higher color fixation rate, and better antibacterial performance compared to the fabric / yarn prepared by the comparative examples. From the data in Table 2, the fabric / yarn prepared by Examples 1-4 of the present application has better fastness.

[0070] The above-described examples are merely examples listed for the purpose of clearly illustrating the present application, so as to facilitate a specific and detailed understanding of the technical solutions of the present application, but are not a limitation on the scope of protection of the present application. For those skilled in the art, without departing from the concept of the present application, a number of modifications and improvements can be made, and the technical solutions obtained by logical analysis, reasoning or limited experiments are within the scope of protection of the appended claims of the present application.

Claims

1. A method for treating dyed cellulosic fiber products against irreversible color change, characterized in that It comprises the following steps: (1) Pretreatment of cellulose fiber products The cellulose fiber products are pretreated with a pretreatment agent before use; (2) Dyeing of cellulose fiber products Sodium sulfate and soda ash are added during the dyeing process, and post-treatment is performed after dyeing; (3) Amination treatment Different equipment is used for amination treatment of cellulose fiber products according to the type of the products, and an amine compound and a fatty alcohol polyoxyethylene ether emulsifier are added to the equipment, then the temperature is raised for treatment, and then the cellulose fiber yarn or fabric after amination treatment is washed with hot water; The dye used in step (2) is a reactive dye with double active groups or multiple active groups; The amine compound used in step (3) is one of high molecular amine compound FR or alkyl amine preparation AIX or a mixture of the two; The amination treatment process of cellulose fiber products in step (3) is as follows: the amount of amine compound is 2-30 g / L, the amount of fatty alcohol polyoxyethylene ether emulsifier is 0.5-1.5 g / L, the treatment temperature is 70-120℃, and the treatment time is 15-60 min.

2. The process for the irreversible color changeless treatment of dyed cellulosic fiber products according to claim 1, characterized in that, The cellulose fiber product is one or more than two kinds of blended yarn or fabric of cotton fiber, Tencel fiber, flax fiber, viscose fiber, bamboo fiber, the fineness of the yarn is 6-60 tex, the mass of the cone yarn is 0.3-1.0 kg, and the fabric has a grammage of 100-280 g / m 2 .

3. The process for the irreversible color changeless treatment of dyed cellulosic fiber products according to claim 1, characterized by, The mass ratio of cellulose fiber products to water during pretreatment, dyeing treatment, post-treatment, and amination treatment is 1: (6-20).

4. The process for the irreversible color changeless treatment of dyed cellulosic fiber products according to claim 1, characterized by, The pretreatment of cellulose fiber products in step (1) uses a pretreatment agent, the amount of fatty alcohol polyoxyethylene ether emulsifier is 0.5-1.5 g / L, the amount of refining agent is 1-2 g / L, the amount of deoiling agent is 0.5-2 g / L, the treatment temperature is 85-100℃, and the treatment time is 10-20 min.

5. The method for treating dyed cellulosic fiber products according to claim 1, wherein The process conditions for dyeing of cellulose fiber products in step (2) are as follows: the dyeing temperature is 50-90℃, the dyeing time is 40-60 min, the amount of sodium sulfate is 10-80 g / L, and the amount of soda ash is 4-25 g / L.

6. The method for treating dyed cellulosic fiber products according to claim 1, wherein The process conditions for post-treatment of dyeing in step (2) are as follows: the amount of soaping agent is 2-8 g / L, the soaping temperature is 80-100℃, the soaping time is 10-20 min, then hot water washing is performed, and the hot water washing temperature and time are the same as the soaping temperature and time.

7. The process for the irreversible color changeless treatment of dyed cellulosic fiber products according to claim 2, characterized by, The amination treatment in step (3) is performed on a cheese dyeing machine for yarn amination treatment, and on an overflow dyeing machine or a tenter for fabric amination treatment, the pump speed of the cheese dyeing machine is set to 80-98%, the cloth speed of the overflow dyeing machine is 200-260 m / min, and the rolling rate of the tenter is 65-80%.

Citation Information

Patent Citations

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