Stain-resistant linen fabric and preparation method thereof

Abstract

The invention provides a stain-resistant linen fabric and a preparation method thereof, and belongs to the technical field of linen fabrics, the preparation method comprises the following steps: S1, cleaning linen fibers, soaking the cleaned linen fibers in a composite bulking solution for 20-25 min, and carrying out subsequent treatment to obtain pretreated fibers; the composite leavening liquid comprises a leavening agent and perfluorohexyl ethyl acrylate; s2, blending the pretreated fibers with oleophobic fibers to obtain yarns; s3, weaving the yarns to obtain a blank fabric; s4, performing first treatment on the blank fabric by using a refining agent solution to obtain a first treated fabric; carrying out secondary treatment on the first treated fabric by using a post-treatment solution; and finally, shaping to obtain the stain-resistant linen fabric. The post-treatment liquid is prepared from vinyl terminated polydimethylsiloxane and a polyether type polyurethane prepolymer. The oil stain resistance and the water stain resistance of the prepared linen fabric can be improved at the same time.

Description

Technical Field

[0001] The present invention belongs to the technical field of linen fabrics, and particularly relates to a stain-resistant linen fabric and a preparation method thereof. Background Art

[0002] Linen fabrics are products made from linen fibers. Currently, the commonly used linen fibers are all taken from the stem bark of high-quality hemp plants and are extracted through complex processes. Such fiber materials have a long development history in China. Linen fabrics are also called crow hemp and flax. Due to their good hygroscopicity, fast moisture conduction, and relatively fine diameter, they are one of the main fiber raw materials for spring and summer clothes. Generally, the cloth woven from linen fibers is called linen fabric. After blending linen fibers with other fibers, the comfort of the fabric can be improved. Such fabrics have important applications in fields such as handkerchiefs, shirt fabrics, crepe silk, fancy colored yarns, sportswear, curtains, wall coverings, tablecloths, and bedding.

[0003] Linen fibers are short and thick, with natural knots and a texture on the surface. The fibers are in a bundle structure, with high strength but easy to bend, resulting in the fabric being prone to wrinkling and needing to be ironed to restore flatness after washing. Linen is widely used in summer clothing, home textiles, and environmental protection packaging fields due to its properties such as breathability, anti-static, and antibacterial.

[0004] In terms of stain resistance, the surface of linen fibers lacks oleophobic groups, and oily stains are easily infiltrated into the fiber gaps through capillary action, forming stubborn stains. Moreover, due to the polar groups and pore structure of linen fibers, it has hydrophilicity (water contact angle < 90°), resulting in water-based stains being easily adsorbed quickly and diffused into the fiber interior, and it is difficult to completely remove them through conventional cleaning. Summary of the Invention

[0005] To solve the problems in the background art, the present invention provides a stain-resistant linen fabric and a preparation method thereof, which can improve the oil stain resistance and water stain resistance of the obtained linen fabric.

[0006] To achieve the above object, in the first aspect, the present invention provides a preparation method of a stain-resistant linen fabric, including the following steps:

[0007] S1. After the linen fibers are cleaned, they are soaked in a composite bulking agent solution for 20 - 25 minutes, and then through subsequent treatment, pretreated fibers are obtained; the composite bulking agent solution includes a bulking agent and perfluorohexylethyl acrylate;

[0008] S2. The pretreated fibers obtained in S1 are blended with oleophobic fibers to obtain yarns;

[0009] S3. The yarns obtained in S2 are woven to obtain a rough fabric;

[0010] S4. First, use a refining agent solution to perform the first treatment on the blank fabric to obtain a first-treated fabric; then use a post-treatment liquid to perform the second treatment on the first-treated fabric; finally, perform shaping to obtain the stain-resistant linen fabric; the post-treatment liquid includes vinyl-terminated polydimethylsiloxane and polyether-type polyurethane prepolymer.

[0011] Further, in S1, the concentration of the bulking agent in the composite bulking liquid is 3.2 - 3.5 g / L; the concentration of perfluorohexylethyl acrylate is 4.5 - 5 g / L.

[0012] Further, in S2, the oil-repellent fiber is made of polypropylene fiber.

[0013] Further, in S2, the blending ratio of the pretreated fiber to the oil-repellent fiber is 6:(1.5 - 1.8).

[0014] Further, in S4, the concentration of the refining agent solution is 1 - 3 g / L.

[0015] Further, in S4, the specific operation of the first treatment is as follows: first immerse the blank fabric in the refining agent solution, control the liquor ratio to 60 - 80%; then pre-dry at 80 - 90 °C for 5 - 8 min, and then wash with water at 40 - 50 °C to remove residual impurities and unreacted chemical substances.

[0016] Further, in S4, the mass fraction of vinyl-terminated polydimethylsiloxane in the post-treatment liquid is 6 - 8%, and the mass fraction of polyether-type polyurethane prepolymer is 9 - 12%.

[0017] Further, in S4, the specific operation of the second treatment is as follows: first immerse the first-treated fabric in the post-treatment liquid, control the impregnation time to 12 - 15 min; then cure at 120 - 130 °C for 12 - 15 min.

[0018] In the second aspect, the present invention provides a stain-resistant linen fabric prepared by the above preparation method.

[0019] This application has the following beneficial effects:

[0020] The present invention uses a composite bulking liquid, which includes a bulking agent and perfluorohexylethyl acrylate. The bulking treatment increases the fiber gaps and forms a porous structure. The high porosity caused by the bulking treatment and the weak hydrophobicity of the short-chain fluorocarbon (perfluorohexylethyl acrylate) are superimposed. While the fluorocarbon layer cannot completely cover the pores, the water absorption channels increase instead;

[0021] On this basis, a post-treatment liquid is added, which contains vinyl-terminated polydimethylsiloxane and polyether-type polyurethane prepolymer. On the one hand, the low surface energy property of vinyl-terminated polydimethylsiloxane can further reduce the affinity between fibers and water and inhibit capillary water absorption. On the other hand, vinyl-terminated polydimethylsiloxane can form an elastic hydrophobic film, fill the pores exposed after fluffing treatment, and combine with the weak hydrophobic layer of short-chain fluorocarbon (perfluorohexylethyl acrylate) to form a denser waterproof barrier, thereby achieving the effect of synergistically improving the water stain resistance / water repellency performance.

[0022] Meanwhile, on the one hand, in the high-porosity region of the fluffy fibers, the polyether-type polyurethane prepolymer can form a three-dimensional network structure to partially close the pores. On the other hand, the polyether-type polyurethane prepolymer fixes the short-chain fluorocarbon (perfluorohexylethyl acrylate) and vinyl-terminated polydimethylsiloxane through chemical bonds, thereby synergistically enhancing the overall water repellency performance and water repellency durability. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 、Comparison trend chart of the oil repellency grade test data of the stain-resistant linen fabrics prepared in Examples 1-3 and Comparative Examples 1-3 in the test examples of the present invention;

[0024] Figure 2 、Comparison trend chart of the water contact angle test data of the stain-resistant linen fabrics prepared in Examples 1-3 and Comparative Examples 1-3 in the test examples of the present invention. DETAILED DESCRIPTION OF THE INVENTION

[0025] The following further describes the present application in detail with reference to the examples.

[0026] The raw materials of the examples and comparative examples of the present application are all commercially available except as otherwise specified.

[0027] Example 1: A method for preparing a stain-resistant linen fabric, comprising the following steps:

[0028] S1. After the linen fibers are subjected to a cleaning treatment, they are soaked in a composite fluffing liquid for 22 min, and then subjected to subsequent treatment to obtain pretreated fibers.

[0029] The cleaning treatment specifically includes: ① soaking in a sulfuric acid aqueous solution (concentration: 2 g / L) at 45 °C for 40 min and then washing with water; ② soaking in a mixed aqueous solution (mass fraction of sodium hydroxide: 3%, mass fraction of hydrogen peroxide: 4%) at 90 °C for 90 min and then washing with water; ③ beating the fibers; ④ soaking in a sulfuric acid aqueous solution (concentration: 0.5 g / L) for 5 min and then washing with water.

[0030] The composite leavening liquid includes a leavening agent, perfluorohexylethyl acrylate, and ethyl acetate. Among them, the leavening agent HS-620 was purchased from Zhongshan Hongsheng Biotechnology Co., Ltd., and the concentration of the leavening agent in the composite leavening liquid is 3.3 g / L. The concentration of perfluorohexylethyl acrylate is 4.8 g / L. Perfluorohexylethyl acrylate was purchased from Wuhan Huaxiang Kejie Biotechnology Co., Ltd.

[0031] The subsequent treatments are all steps of existing technologies, including successively: water washing, dehydration, oiling, de-oiling water, drying, cutting, and mechanical loosening.

[0032] S2. Blending the pretreated fibers obtained in S1 and polypropylene fibers according to a blending ratio of 6:1.7 to obtain yarns.

[0033] S3. Weaving the yarns obtained in S2 to obtain a blank fabric.

[0034] S4. First, use a refining agent solution to conduct the first treatment on the blank fabric. The specific operation of the first treatment is: first immerse the blank fabric in the refining agent solution, control the liquor ratio to 70%, and ensure that the solution fully penetrates the fiber pores; then pre-dry at 85°C for 7 min, and then wash with warm water at about 45°C to remove residual impurities and unreacted chemical substances to obtain the first-treated fabric. The concentration of the refining agent solution is 3 g / L. The refining agent is the Taiyang New Material TY1-21 low-temperature refining agent, purchased from Dongguan Taiyang New Material Technology Co., Ltd.

[0035] Then use a post-treatment liquid to conduct the second treatment on the first-treated fabric. The specific operation of the second treatment is: first immerse the first-treated fabric in the post-treatment liquid, control the impregnation time to 13 min; then cure at 125°C for 13 min; finally, shape it to obtain the stain-resistant linen fabric. The post-treatment liquid includes vinyl-terminated polydimethylsiloxane, polyether-type polyurethane prepolymer, and a mixed solvent. The mixed solvent is obtained by mixing ethyl acetate and N,N-dimethylformamide according to a mass ratio of 5:1. Among them, vinyl-terminated polydimethylsiloxane was purchased from Wuhan Lanabai Pharmaceutical and Chemical Co., Ltd., and the mass fraction of vinyl-terminated polydimethylsiloxane is 7%. The polyether-type polyurethane prepolymer (Se-725) was purchased from Foshan Yujiaxuan Chemical Co., Ltd., and the mass fraction of the polyether-type polyurethane prepolymer is 10%.

[0036] Example 2: The difference between this example and Example 1 lies in: A method for preparing a stain-resistant linen fabric, including the following steps:

[0037] S1. After the flax fibers are cleaned, they are soaked in the composite swelling solution for 25 minutes and then subjected to subsequent treatment to obtain pretreated fibers. The composite swelling solution includes a swelling agent, perfluorohexylethyl acrylate, and ethyl acetate. Among them, the swelling agent HS-620 is purchased from Zhongshan Hongsheng Biotechnology Co., Ltd., and the concentration of the swelling agent in the composite swelling solution is 3.2 g / L. The concentration of perfluorohexylethyl acrylate is 4.5 g / L.

[0038] S2. The pretreated fibers obtained in S1 are blended with polypropylene fibers at a blending ratio of 6:1.5 to obtain yarns.

[0039] S3. The yarns obtained in S2 are woven to obtain a blank fabric.

[0040] S4. First, the blank fabric is subjected to a first treatment with a refining agent solution. The specific operation of the first treatment is as follows: First, the blank fabric is immersed in the refining agent solution, and the liquor ratio is controlled at 60%, ensuring that the solution fully penetrates the fiber pores; then it is pre-dried at 80°C for 8 minutes, and then washed with water at 40°C to remove residual impurities and unreacted chemical substances to obtain a first-treated fabric. The concentration of the refining agent solution is 3 g / L. The refining agent is the Taiyang New Material TY1-21 low-temperature refining agent, purchased from Dongguan Taiyang New Material Technology Co., Ltd.

[0041] Then, the first-treated fabric is subjected to a second treatment with a post-treatment solution. The specific operation of the second treatment is as follows: First, the first-treated fabric is immersed in the post-treatment solution, and the impregnation time is controlled for 15 minutes; then it is cured at 120°C for 15 minutes; finally, it is shaped to obtain the stain-resistant flax fabric. The post-treatment solution includes vinyl-terminated polydimethylsiloxane, polyether-type polyurethane prepolymer, and a mixed solvent, and the mixed solvent is obtained by mixing ethyl acetate and N,N-dimethylformamide in a mass ratio of 5:1. Among them, the mass fraction of vinyl-terminated polydimethylsiloxane is 6%, and the mass fraction of polyether-type polyurethane prepolymer is 9%.

[0042] Example 3: The difference between this example and Example 1 is: A method for preparing a stain-resistant flax fabric, including the following steps:

[0043] S1. After the flax fibers are cleaned, they are soaked in the composite swelling solution for 20 minutes and then subjected to subsequent treatment to obtain pretreated fibers. The composite swelling solution includes a swelling agent, perfluorohexylethyl acrylate, and ethyl acetate. Among them, the swelling agent HS-620 is purchased from Zhongshan Hongsheng Biotechnology Co., Ltd., and the concentration of the swelling agent in the composite swelling solution is 3.5 g / L. The concentration of perfluorohexylethyl acrylate is 5 g / L.

[0044] S2. The pretreated fibers obtained in S1 are blended with polypropylene fibers at a blending ratio of 6:1.8 to obtain yarns.

[0045] S3. Weave the yarn obtained in S2 to get a rough fabric.

[0046] S4. First, use a scouring agent solution to conduct the first treatment on the rough fabric. The specific operation of the first treatment is as follows: First, immerse the rough fabric in the scouring agent solution, control the liquor ratio at 80%, and ensure that the solution fully penetrates the fiber pores; then pre-dry at 90 °C for 5 min, and subsequently wash with water at 50 °C to remove residual impurities and unreacted chemical substances, obtaining a first-treated fabric. The concentration of the scouring agent solution is 3 g / L. The scouring agent is the Taiyang New Material TY1-21 low-temperature scouring agent, purchased from Dongguan Taiyang New Material Technology Co., Ltd.

[0047] Then, use a post-treatment liquid to conduct the second treatment on the first-treated fabric. The specific operation of the second treatment is as follows: First, immerse the first-treated fabric in the post-treatment liquid, control the impregnation time at 12 min; then cure at 130 °C for 12 min; finally, perform shaping to obtain a stain-resistant linen fabric. The post-treatment liquid includes vinyl-terminated polydimethylsiloxane, polyether-type polyurethane prepolymer, and a mixed solvent. The mixed solvent is obtained by mixing ethyl acetate and N,N-dimethylformamide in a mass ratio of 5:1. Among them, the mass fraction of vinyl-terminated polydimethylsiloxane is 8%, and the mass fraction of polyether-type polyurethane prepolymer is 12%.

[0048] Comparative Example 1: The difference between this comparative example and Example 1 is that in the preparation of the composite bulking agent, perfluorohexylethyl acrylate is deleted; and the post-treatment liquid is deleted.

[0049] Specifically, a method for preparing a stain-resistant linen fabric includes the following steps:

[0050] S1. After the linen fibers are cleaned, soak them in the composite bulking agent for 22 min, and then through subsequent treatment to obtain pretreated fibers. The composite bulking agent includes a bulking agent and ethyl acetate. Among them, the bulking agent HS-620 is purchased from Zhongshan Hongsheng Biotechnology Co., Ltd., and the concentration of the bulking agent in the composite bulking agent is 3.3 g / L.

[0051] S2. Blend the pretreated fibers obtained in S1 with polypropylene fibers according to a blending ratio of 6:1.7 to obtain yarn.

[0052] S3. Weave the yarn obtained in S2 to get a rough fabric.

[0053] S4. The first treatment of the blank fabric is carried out with a refining agent solution. The specific operation of the first treatment is as follows: First, immerse the blank fabric in the refining agent solution, control the liquor ratio at 70%, and ensure that the solution fully penetrates the fiber pores; then pre-dry at 85 °C for 7 min, and then wash with warm water at about 45 °C to remove residual impurities and unreacted chemical substances, obtaining the first-treated fabric. The concentration of the refining agent solution is 3 g / L. Then perform shaping to obtain the stain-resistant linen fabric.

[0054] Comparative Example 2: The difference between this comparative example and Example 1 is that the post-treatment liquid is deleted.

[0055] Comparative Example 3: The difference between this comparative example and Example 1 is that in the preparation of the composite bulking agent, perfluorohexylethyl acrylate is deleted.

[0056] Test Example: Test object: The stain-resistant linen fabrics prepared in Examples 1 - 3 and Comparative Examples 1 - 3. Test items: ① Stain resistance to water stains / water repellency - water contact angle; ② Stain resistance to oil stains / oil repellency (grade): AATCC118 - 2018 "Test for Oil Repellency: Resistance to Hydrocarbons". Test results: See Table 1.

[0057] Table 1. Test data of the test example

[0058] Oil repellency level / grade Water contact angle / ° Example 1 6 91 Example 2 6 92 Example 3 6 92 Comparative example 1 5 85 Comparative example 2 6 81 Comparative example 3 5 87

[0059] Result analysis: Analyzing Examples 1 - 3 and combining with the data in Table 1 and Figure 1 - Figure 2 , it can be seen that the oil repellency grade of the stain-resistant linen fabric prepared by the present invention (Examples 1 - 3) reaches level 6, and the water contact angle reaches more than 91°. It shows that the stain-resistant linen fabric prepared by the present invention (Examples 1 - 3) has both excellent stain resistance to oil stains / oil repellency and stain resistance to water stains / water repellency.

[0060] Analyzing Example 1 and Comparative Examples 1 - 3 and combining with the data in Table 1 and Figure 1 - Figure 2 , by comparing Comparative Example 1 and Comparative Example 2, it can be known that compared with Comparative Example 1, perfluorohexylethyl acrylate is added in the preparation of the composite bulking agent used in Comparative Example 2. As a result, the oil repellency grade of the linen fabric prepared rises from level 5 (Comparative Example 1) to level 6 (Comparative Example 2), and the water contact angle drops from 85° (Comparative Example 1) to 81° (Comparative Example 2). It shows that adding perfluorohexylethyl acrylate alone can improve the stain resistance to oil stains / oil repellency of the prepared linen fabric, but at the same time, it will also cause the stain resistance to water stains / water repellency of the prepared linen fabric to decrease instead of increase.

[0061] This is because, on the one hand, when the bulking agent is soaked, short-chain fluorocarbons (perfluorohexylethyl acrylate) are introduced, which can reduce the surface energy of the fiber, form an oil-repellent layer, and improve the oil resistance. On the other hand, after the original linen is bulking-treated, the fiber gaps will increase, forming a porous structure. Moisture penetrates quickly through capillary action, enhancing the water absorption, while the water repellency decreases. The superposition of the high porosity caused by the bulking treatment and the weak hydrophobicity of the short-chain fluorocarbons (perfluorohexylethyl acrylate) results in an increase in the water absorption channels instead of the fluorocarbon layer completely covering the pores, further reducing the water repellency.

[0062] By comparing Comparative Example 1 and Comparative Example 3, it can be seen that compared with Comparative Example 1, the use of the post-treatment liquid is increased in Comparative Example 3, and the result is that the oil repellency grade of the linen fabric prepared remains unchanged, and the water contact angle increases from 85° (Comparative Example 1) to 87° (Comparative Example 3). This shows that simply increasing the use of the post-treatment liquid (containing vinyl-terminated polydimethylsiloxane and polyether-type polyurethane prepolymer) can improve the water stain resistance / water repellency of the prepared linen fabric.

[0063] Combined with Example 1 for comparison, it can be seen that adding perfluorohexylethyl acrylate to the composite bulking liquid and increasing the use of the post-treatment liquid (containing vinyl-terminated polydimethylsiloxane and polyether-type polyurethane prepolymer) can produce a synergistic effect, ensuring excellent oil stain resistance / oil repellency of the prepared linen fabric while synergistically improving the water stain resistance / water repellency of the prepared linen fabric.

[0064] In addition, it should be noted that in the above specific embodiments, the various specific technical features described can be combined in any suitable manner without contradiction. To avoid unnecessary repetition, the present invention will not separately describe various possible combination methods.

[0065] In addition, any combination can be made between various different embodiments of the present invention as long as it does not violate the idea of the present invention, and it should also be regarded as the content disclosed by the present invention.

Claims

1. A method for preparing a stain-resistant linen fabric, characterized in that: It includes the following steps: S1. After the linen fiber is subjected to cleaning treatment, it is soaked in the composite bulking agent solution for 20 - 25 min, and then through subsequent treatment, the pretreated fiber is obtained; the composite bulking agent solution includes a bulking agent and perfluorohexylethyl acrylate; S2. The pretreated fiber obtained in S1 is blended with oil-repellent fiber to obtain yarn; S3. The yarn obtained in S2 is woven to obtain a blank fabric; S4. First, the blank fabric obtained in S3 is subjected to the first treatment with a refining agent solution to obtain a first-treated fabric; then the first-treated fabric is subjected to the second treatment with a post-treatment solution; finally, shaping is carried out to obtain the stain-resistant linen fabric; the post-treatment solution includes vinyl-terminated polydimethylsiloxane and polyether-type polyurethane prepolymer.

2. The preparation method of the stain-resistant linen fabric according to claim 1, characterized in that, In S1, the concentration of the bulking agent in the composite bulking agent solution is 3.2 - 3.5 g / L; the concentration of perfluorohexylethyl acrylate is 4.5 - 5 g / L.

3. The method for preparing the stain-resistant linen fabric according to claim 1, wherein: In S2, the oil-repellent fiber is made of polypropylene fiber.

4. The method for preparing the stain-resistant linen fabric according to claim 1 or 3, characterized in that: In S2, the blending ratio of the pretreated fiber to the oil-repellent fiber is 6:(1.5 - 1.8).

5. The preparation method of the stain-resistant linen fabric according to claim 1, wherein, In S4, the concentration of the refining agent solution is 1 - 3 g / L.

6. The method for preparing the stain-resistant linen fabric according to claim 1 or 5, characterized in that: In S4, the specific operation of the first treatment is: first immerse the blank fabric in the refining agent solution, control the liquor ratio to be 60 - 80%; then pre-dry at 80 - 90 °C for 5 - 8 min, and subsequently wash with water at 40 - 50 °C.

7. The method for preparing the stain-resistant linen fabric according to claim 1, characterized in that: In S4, the mass fraction of vinyl-terminated polydimethylsiloxane in the post-treatment solution is 6 - 8%, and the mass fraction of polyether-type polyurethane prepolymer is 9 - 12%.

8. The preparation method of the stain-resistant linen fabric according to claim 1 or 7, characterized in that, In S4, the specific operation of the second treatment is: first immerse the first-treated fabric in the post-treatment solution, control the impregnation time to be 12 - 15 min; then cure at 120 - 130 °C for 12 - 15 min.

9. A stain-resistant linen fabric, characterized in that: It is prepared by using the preparation method according to any one of claims 1 - 8.

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