An oil-proof and stain-proof denim fabric and its preparation method

Abstract

The present invention provides an anti-oil and anti-stain denim fabric and a preparation method thereof, which relates to the technical field of fabric finishing and processing. The preparation method of the anti-oil and anti-stain denim fabric of the present invention adopts the padding method, and uses an anti-oil and anti-stain finishing agent to treat the denim fabric, and after the treatment is completed, baking is carried out to obtain the anti-oil and anti-stain denim fabric. The anti-oil and anti-stain finishing agent of the present invention includes raw materials such as fluorinated emulsion, organic acid, softener, penetrant, water, etc., wherein the fluorinated emulsion is perfluorohexylethyl methacrylate. The present invention overcomes the problems such as poor wash resistance of the fabric after finishing with short fluorocarbon chain fabric finishing agents, and realizes the preparation of low-cost anti-oil and anti-stain denim fabrics.

Description

Technical Field

[0001] The present invention relates to the technical field of fabric finishing and processing, and particularly to an oil-proof and stain-proof denim fabric and a preparation method thereof. Background Art

[0002] Denim is a very popular fabric, widely used in making clothing such as jeans and jackets. It is usually made of cotton, with durability and a unique texture. With the wide use of denim fabric, and in order to meet the requirements in terms of the practicality, extended service life, meeting consumer needs and environmental protection of denim fabric, the oil-proof and stain-proof denim fabric has emerged as the times require.

[0003] Fluorinated fabric finishing agents are important materials in textile post-finishing. Fabrics treated with them can exhibit excellent water and oil repellency properties. Fluorinated finishing agents are widely used in fabric finishing because of their high efficiency at low concentrations, low required adhesion energy, and their ability to maintain characteristics such as the soft handfeel, breathability and moisture retention of the fabric.

[0004] Among fluorinated fabric finishing agents, longer fluorocarbon chains have stronger fluidity, and the polymers are prone to crystallization, endowing the material with good hydrophobic and oleophobic properties. However, these compounds accumulate in the environment and organisms, bringing potential risks. Compared with fluorinated polymers with long fluorocarbon chains, raw materials with short fluorocarbon chains have good degradability. However, different from long fluorocarbon chains, short fluorocarbon chains have poor crystallinity, are difficult to migrate and stably arrange on the material surface, and have poor adhesion, resulting in their easy shedding. Therefore, although a fabric finishing agent with short fluorocarbon chains can be used to prepare a fabric with good water and oil repellency effects, the wash resistance of the fabric is often poor, and the product performance drops significantly after several washes, unable to meet the actual use requirements.

[0005] Therefore, how to overcome the problems existing in the existing fabric finishing agents with short fluorocarbon chains and realize the preparation of an oil-proof and stain-proof denim fabric with good wash resistance is of great significance for improving the practicality of denim fabric, extending its service life, meeting consumer needs and environmental protection requirements. Summary of the Invention

[0006] To solve the above problems, the present invention provides an oil-proof and stain-proof denim fabric and a preparation method thereof. By adjusting the types of raw materials of the oil-proof and stain-proof finishing agent and the ratio between the raw materials, and combining with a specific treatment process, the present invention significantly improves the wash resistance of the fabric while enhancing the oil-proof and stain-proof performance of the denim fabric.

[0007] The preparation method of the oil-proof and stain-proof denim fabric of the present invention is as follows:

[0008] Using the padding method, treat the denim fabric with the oil-proof and stain-proof finishing agent, and bake it after the treatment is completed to obtain the oil-proof and stain-proof denim fabric.

[0009] Further, the padding method is two - dip and two - nip, and the liquor - pickup rate is 50% - 90%. Preferably, the liquor - pickup rate is 75%.

[0010] Further, the baking is carried out in two steps. First, the treated denim fabric is pre - baked at 100°C - 110°C for 3.5 - 5 min, and then baked at 160°C - 180°C for 1 - 2 min to complete the baking. Preferably, the pre - baking temperature is 100°C, the pre - baking time is 5 min, the baking temperature is 180°C, and the baking time is 1 min.

[0011] Further, the oil - and - stain repellent finishing agent comprises the following raw materials in weight percentages:

[0012] Fluorinated emulsion 20% - 40%, organic acid 5% - 15%, softener 5% - 10%, penetrant 1% - 5%, glycerol 5% - 20%, and the balance is water.

[0013] Preferably, the oil - and - stain repellent finishing agent comprises the following raw materials in weight percentages:

[0014] Fluorinated emulsion 30%, organic acid 15%, softener 5%, penetrant 2%, glycerol 20%, and the balance is water.

[0015] Further, the fluorinated emulsion is perfluorohexylethyl methacrylate.

[0016] Further, the organic acid is one or more of citric acid, malic acid, tartaric acid, and oxalic acid. Preferably, the organic acid is one or more of citric acid, malic acid, and tartaric acid. More preferably, the organic acid is composed of citric acid, malic acid, and tartaric acid in a molar ratio of (3 - 5):(1 - 2):(1 - 2). Further preferably, the organic acid is composed of citric acid, malic acid, and tartaric acid in a molar ratio of 5:1:1.

[0017] Further, the softener is an organosilicon softener.

[0018] Further, the penetrant is a non - ionic surfactant. Preferably, the penetrant is fatty alcohol polyoxyethylene ether.

[0019] The present invention also provides an oil - and - stain repellent denim fabric prepared according to the above method.

[0020] Compared with the prior art, the beneficial technical effects of the present invention are:

[0021] Through the cross - linking effect of the fluorinated emulsion and the organic acid, the present invention improves the wash - resistance and oil - and - stain repellent performance of the oil - and - stain repellent denim fabric, and overcomes the problem of poor wash - resistance (including water - wash resistance and detergent - wash resistance) of the fabric after finishing with a short fluorocarbon - chain fabric finishing agent.

[0022] By adding glycerol, the present invention increases the intermolecular force between the finishing agent and the fabric, and improves the adhesion of the fluorinated emulsion and the organic acid to the fabric.

[0023] By using a composite organic acid, the present invention adjusts the number of carboxyl groups in the finishing agent, realizes the regulation of the crosslinking density, balances the oil and stain resistance and flexibility of the material, and avoids the deterioration of the hand feeling of the denim fabric.

[0024] By using a softening agent and a penetrant, the present invention alleviates to a certain extent the adverse effect of the oil and stain resistance finishing on the air permeability of the denim fabric, so that the denim fabric has good air permeability while also having a certain air permeability.

[0025] The present invention adopts a step-by-step baking process to remove excess moisture and solvents, ensure the uniform distribution of the oil and stain resistance finishing agent, ensure sufficient crosslinking, and effectively improve the oil and stain resistance performance of the denim fabric.

[0026] The preparation method provided by the present invention is simple and fast, does not require complex raw material synthesis steps, and a variety of functional additives are widely available and low in price, thereby reducing the cost of oil and stain resistance treatment of denim fabrics and realizing the preparation of low-cost oil and stain resistance denim fabrics. Specific Embodiments

[0027] The present invention provides a method for preparing an oil and stain resistance denim fabric, and the specific steps are as follows:

[0028] Using the padding method, treat the denim fabric with an oil and stain resistance finishing agent, and bake after the treatment is completed to obtain an oil and stain resistance denim fabric.

[0029] In an embodiment 1, the padding method is two-bath two-padding, and the pick-up rate is 50% - 90%.

[0030] In an embodiment 1, the pick-up rate is 75%.

[0031] In an embodiment 1, the baking is carried out in two steps. First, pre-bake the treated denim fabric at 100°C - 110°C for 3.5 - 5 minutes, and then bake at 160°C - 180°C for 1 - 2 minutes to complete the baking.

[0032] In an embodiment 1, the pre-baking temperature is 100°C, the pre-baking time is 5 minutes, the baking temperature is 180°C, and the baking time is 1 minute.

[0033] The pre-baking stage of the present invention is the stage where the cross-linking reaction mainly occurs, so a relatively low temperature compared to the formal baking is selected for this stage. At the same time, the pre-baking time is longer than that of the baking treatment, and its purpose is also to ensure the full progress of the cross-linking reaction. After the pre-baking is completed, the temperature is increased to perform the baking treatment on the denim fabric, which can not only completely remove the solvent, but also enhance the stability and durability of the anti-oil and stain layer, thereby effectively improving the anti-oil and stain performance of the denim fabric.

[0034] In Example 1, the anti-oil and stain finishing agent comprises raw materials in the following weight percentages:

[0035] Fluorinated emulsion 20% - 40%, organic acid 5% - 15%, softener 5% - 10%, penetrant 1% - 5%, glycerol 5% - 20%, and the balance is water.

[0036] In Example 1, the anti-oil and stain finishing agent comprises raw materials in the following weight percentages:

[0037] Fluorinated emulsion 30%, organic acid 15%, softener 5%, penetrant 2%, glycerol 20%, and the balance is water.

[0038] In Example 1, the fluorinated emulsion is perfluorohexylethyl methacrylate.

[0039] Polymers containing perfluoro groups are mostly fluorocarbon chains (carbon atom number ≥ 8). This is because longer fluorocarbon chains have stronger fluidity, the polymers are easy to crystallize, and the -CF3 groups with lower surface energy are easy to migrate to the surface, making the material have good hydrophobic and oleophobic properties. However, these compounds accumulate in the environment and organisms, bringing potential risks. Compared with fluorinated polymers with long fluorocarbon chains, raw materials with short fluorocarbon chains (carbon atom number ≤ 6) have good degradability. Therefore, the present invention selects perfluorohexylethyl methacrylate (fluorocarbon chain carbon atom number = 6) as the fluorinated emulsion for the anti-oil and stain finishing of denim fabric.

[0040] In Example 1, the organic acid is one or more of citric acid, malic acid, tartaric acid, and oxalic acid.

[0041] In Example 1, the organic acid is one or more of citric acid, malic acid, and tartaric acid.

[0042] In Example 1, the organic acid is composed of citric acid, malic acid, and tartaric acid in a molar ratio of (3 - 5):(1 - 2):(1 - 2).

[0043] In Example 1, the organic acid is composed of citric acid, malic acid, and tartaric acid in a molar ratio of 5:1:1.

[0044] As is well known, different from long fluorocarbon chains, short fluorocarbon chains have poor crystallinity, are difficult to migrate and stably arrange on the material surface, and have poor adhesion, resulting in insufficient hydrophobic and oleophobic effects. Therefore, in the finishing agent of the present invention, a compound organic acid and glycerol are used. Among them, glycerol can play a role in stabilizing and dispersing. In addition, the hydrogen bond between the hydroxyl groups in glycerol and the hydroxyl groups on the cellulose macromolecules increases the intermolecular force, further improving the adhesion of the fluorinated emulsion on the denim fabric, and then improving the washability of the oil-proof and stain-proof denim fabric. In addition, glycerol can increase the average length and degree of branching of cross-linking, and improve the flexibility of the fabric.

[0045] At the same time, the present invention strictly limits the composition and ratio of the organic acid.

[0046] Citric acid has a multi-carboxyl structure, malic acid has a dicarboxyl structure, and tartaric acid has a dicarboxyl and hydroxyl structure. The present invention mainly uses citric acid, and by compounding a small amount of malic acid and tartaric acid, the contents of carboxyl and hydroxyl groups in the reaction raw materials are adjusted to ensure that under the premise of sufficient cross-linking, partial hydroxyl groups are provided to form hydrogen bonds, further improving the binding degree between the treatment agent and the fabric, and at the same time avoiding too poor air permeability and flexibility of the fabric.

[0047] In an embodiment 1, the softener is an organosilicon softener.

[0048] In an embodiment 1, the penetrant is a non-ionic surfactant.

[0049] In an embodiment 1, the penetrant is fatty alcohol polyoxyethylene ether.

[0050] The technical solution provided by the present invention is further described below in conjunction with embodiments.

[0051] Embodiment 1

[0052] A preparation method of an oil-proof and stain-proof denim fabric comprises the following steps:

[0053] Treat the denim fabric with an oil-proof and stain-proof finishing agent, dip and roll twice, the pick-up rate is 75%, pre-bake at 100 °C for 5 min after treatment, and then bake at 180 °C for 1 min to obtain the oil-proof and stain-proof denim fabric.

[0054] The oil-proof and stain-proof finishing agent is composed of the following raw materials in weight percentages:

[0055] 30% of perfluorohexylethyl methacrylate, 15% of organic acid, 5% of organosilicon softener, 2% of fatty alcohol polyoxyethylene ether, 20% of glycerol, and the balance is water;

[0056] The organic acid is composed of citric acid, malic acid, and tartaric acid in a molar ratio of 5:1:1.

[0057] Example 2

[0058] A preparation method of an oil-proof and stain-proof denim fabric is as follows:

[0059] Treat the denim fabric with an oil-proof and stain-proof finishing agent, dip and roll twice, the liquor pick-up rate is 75%, pre-bake at 100 °C for 5 min after treatment, and then bake at 180 °C for 1 min to obtain the oil-proof and stain-proof denim fabric.

[0060] The oil-proof and stain-proof finishing agent is composed of the following raw materials in weight percentages:

[0061] 20% of perfluorohexylethyl methacrylate, 5% of organic acid, 5% of silicone softener, 1% of fatty alcohol polyoxyethylene ether, 5% of glycerol, and the balance is water;

[0062] The organic acid is composed of citric acid, malic acid, and tartaric acid in a molar ratio of 5:1:1.

[0063] Example 3

[0064] A preparation method of an oil-proof and stain-proof denim fabric is as follows:

[0065] Treat the denim fabric with an oil-proof and stain-proof finishing agent, dip and roll twice, the liquor pick-up rate is 75%, pre-bake at 100 °C for 5 min after treatment, and then bake at 180 °C for 1 min to obtain the oil-proof and stain-proof denim fabric.

[0066] The oil-proof and stain-proof finishing agent is composed of the following raw materials in weight percentages:

[0067] 40% of perfluorohexylethyl methacrylate, 15% of organic acid, 10% of silicone softener, 5% of fatty alcohol polyoxyethylene ether, 20% of glycerol, and the balance is water;

[0068] The organic acid is composed of citric acid, malic acid, and tartaric acid in a molar ratio of 5:1:1.

[0069] Comparative Example 1

[0070] Same as Example 1, the difference is: dip and roll once, the liquor pick-up rate is 75%.

[0071] Comparative Example 2

[0072] Same as Example 1, the difference is: pre-bake at 100 °C for 2 min.

[0073] Comparative Example 3

[0074] Same as Example 1, the difference is: the oil-proof and stain-proof finishing agent does not contain organic acid.

[0075] Comparative Example 4

[0076] Same as Example 1, with the difference that: the anti-oil stain finishing agent does not contain glycerol.

[0077] Comparative Example 5

[0078] Same as Example 1, with the difference that: the glycerol in the anti-oil stain finishing agent is replaced with an equal amount of ethanol.

[0079] Comparative Example 6

[0080] Same as Example 1, with the difference that: the organic acid is citric acid.

[0081] Comparative Example 7

[0082] Same as Example 1, with the difference that: it is composed of citric acid, malic acid, and tartaric acid in a molar ratio of 1:1:1.

[0083] Test Example 1

[0084] Detect the performance of the denim fabrics obtained after finishing the examples and comparative examples. The detection method is as follows:

[0085] Waterproofness: Test according to the method in AATCC-22. On the LFY-214 type water repellency tester, after spraying water, observe the wetting degree of the fabric surface and evaluate the water repellency grade;

[0086] Oil repellency: Test according to the method in AATCC-118. Prepare 8 standard reagents with gradually decreasing surface tensions. Use a dropper to drop various standard test solutions on the fabric surface respectively, observe the wetting degree and evaluate the oil repellency grade:

[0087] Wash resistance: The washing method is carried out according to AATCC-135-2014.

[0088] The detection results are shown in Table 1.

[0089] Table 1 Detection results of denim fabric treatment in examples and comparative examples

[0090]

[0091] Example 4

[0092] A preparation method of an anti-oil stain denim fabric, the steps are as follows:

[0093] Treat the denim fabric with an anti-oil stain finishing agent, dip and roll twice, the liquor pick-up rate is 50%, pre-bake at 100 °C for 5 min after treatment, and then bake at 180 °C for 1 min to obtain the anti-oil stain denim fabric.

[0094] The anti-oil stain finishing agent is composed of the following raw materials in weight percentages:

[0095] 30% perfluorohexylethyl methacrylate, 15% organic acid, 5% silicone softener, 2% fatty alcohol polyoxyethylene ether, 20% glycerol, the balance being water;

[0096] The organic acid consists of citric acid, malic acid and tartaric acid in a molar ratio of 5:1:1.

[0097] Example 5

[0098] A method for preparing an oil-proof and stain-proof denim fabric comprises the following steps:

[0099] Treat the denim fabric with an oil-proof and stain-proof finishing agent by two-dip two-roll padding, with a liquor pickup of 90%. After treatment, pre-bake at 100 °C for 5 min, and then bake at 180 °C for 1 min to obtain the oil-proof and stain-proof denim fabric.

[0100] The oil-proof and stain-proof finishing agent is composed of the following raw materials in weight percentages:

[0101] 30% perfluorohexylethyl methacrylate, 15% organic acid, 5% silicone softener, 2% fatty alcohol polyoxyethylene ether, 20% glycerol, the balance being water;

[0102] The organic acid consists of citric acid, malic acid and tartaric acid in a molar ratio of 5:1:1.

[0103] Example 6

[0104] A method for preparing an oil-proof and stain-proof denim fabric comprises the following steps:

[0105] Treat the denim fabric with an oil-proof and stain-proof finishing agent by two-dip two-roll padding, with a liquor pickup of 50%. After treatment, pre-bake at 110 °C for 3.5 min, and then bake at 180 °C for 1 min to obtain the oil-proof and stain-proof denim fabric.

[0106] The oil-proof and stain-proof finishing agent is composed of the following raw materials in weight percentages:

[0107] 30% perfluorohexylethyl methacrylate, 15% organic acid, 5% silicone softener, 2% fatty alcohol polyoxyethylene ether, 20% glycerol, the balance being water;

[0108] The organic acid consists of citric acid, malic acid and tartaric acid in a molar ratio of 5:1:1.

[0109] Example 7

[0110] A method for preparing an oil-proof and stain-proof denim fabric comprises the following steps:

[0111] The denim fabric is treated with an anti - oil and anti - stain finishing agent by two - dip two - nip, with a liquor pick - up rate of 75%. After treatment, it is pre - baked at 100 °C for 5 min and then baked at 160 °C for 2 min to obtain the anti - oil and anti - stain denim fabric.

[0112] The anti - oil and anti - stain finishing agent is composed of the following raw materials by weight percentage:

[0113] Perfluorohexylethyl methacrylate 30%, organic acid 15%, silicone softener 5%, fatty alcohol polyoxyethylene ether 2%, glycerol 20%, and the balance is water;

[0114] The organic acid is composed of citric acid, malic acid, and tartaric acid in a molar ratio of 5:1:1.

[0115] Example 8

[0116] A method for preparing an anti - oil and anti - stain denim fabric comprises the following steps:

[0117] The denim fabric is treated with an anti - oil and anti - stain finishing agent by two - dip two - nip, with a liquor pick - up rate of 75%. After treatment, it is pre - baked at 100 °C for 5 min and then baked at 180 °C for 1 min to obtain the anti - oil and anti - stain denim fabric.

[0118] The anti - oil and anti - stain finishing agent is composed of the following raw materials by weight percentage:

[0119] Perfluorohexylethyl methacrylate 30%, organic acid 15%, silicone softener 5%, fatty alcohol polyoxyethylene ether 2%, glycerol 20%, and the balance is water;

[0120] The organic acid is composed of citric acid, malic acid, and tartaric acid in a molar ratio of 3:2:2.

[0121] After testing, there is no significant difference in the waterproofness, oil - proofness, and wash resistance of the denim fabrics obtained in Examples 4 - 8 and Examples 1 - 3.

[0122] Specific examples are used in this article to illustrate the principle and implementation mode of the present invention. The descriptions of the above examples are only used to help understand the method and its core idea of the present invention; at the same time, for those of ordinary skill in the art, according to the idea of the present invention, there will be changes in the specific implementation mode and application scope. In summary, the content of this specification should not be construed as a limitation of the present invention.

Claims

1. A preparation method of an anti-oil and anti-stain denim fabric, characterized in that, It includes the following steps: Using the padding method, treat the denim fabric with an anti-oil and anti-stain finishing agent, and bake it after the treatment to obtain the anti-oil and anti-stain denim fabric; The anti-oil and anti-stain finishing agent includes the following raw materials by weight percentage: Fluorinated emulsion 20% - 40%, organic acid 5% - 15%, softener 5% - 10%, penetrant 1% - 5%, glycerol 5% - 20%, and the balance is water; The fluorinated emulsion is perfluorohexylethyl methacrylate; The organic acid is composed of citric acid, malic acid, and tartaric acid in a molar ratio of (3 - 5):(1 - 2):(1 - 2); 2. The preparation method of the anti-oil and anti-stain denim fabric according to claim 1, wherein, The padding method is two-bath two-roll padding, and the liquor pickup is 50% - 90%; 3. The preparation method of the oil-proof denim fabric according to claim 1, characterized in that, The baking is carried out in two steps. First, pre-bake the treated denim fabric at 100°C - 110°C for 3.5 - 5 min, and then bake it at 160°C - 180°C for 1 - 2 min to complete the baking; 4. The preparation method of the oil-proof denim fabric according to claim 3, characterized in that The pre-baking temperature is 100°C, the pre-baking time is 5 min, the baking temperature is 180°C, and the baking time is 1 min; 5. The preparation method of the oil-proof denim fabric according to claim 1, characterized in that The anti-oil and anti-stain finishing agent includes the following raw materials by weight percentage: Fluorinated emulsion 30%, organic acid 15%, softener 5%, penetrant 2%, glycerol 20%, and the balance is water; 6. The preparation method of the oil-proof denim fabric according to claim 1, characterized in that, The softener is an organosilicon softener; 7. The preparation method of the oil-proof denim fabric according to claim 1, characterized in that, The penetrant is a non-ionic surfactant; 8. An anti-oil and anti-stain denim fabric prepared by the method according to any one of claims 1 - 7.

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