A hydrophobic fabric and its preparation method and application

By repeatedly reacting vinyl nitrogen heterocyclic compounds with fluorinated acrylate compounds and acrylamide compounds, and combining crosslinking agents and initiators, the problems of complex processes and insufficient hydrophobic properties in the preparation of traditional hydrophobic fabrics have been solved, realizing the preparation of efficient and environmentally friendly hydrophobic fabrics, which are suitable for a variety of cellulose fabrics.

CN120158929BActive Publication Date: 2025-12-05DONGHUA UNIV +1
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Patent Information

Application Number
CN202510311284.4
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-03-17
Publication Date
2025-12-05
Estimated Expiration
2045-03-17

AI Technical Summary

Technical Problem

Existing hydrophobic fabric preparation technologies suffer from problems such as complex processes, excessive fluorine atom introduction, excessively long fluorine chain length, and insufficient hydrophobic properties, making it difficult to meet the requirements of high-performance application scenarios.

Method used

Vinyl nitrogen heterocyclic compounds are reacted with fluorinated acrylate compounds and acrylamide compounds in an inert gas atmosphere through multiple contact reactions. Combined with crosslinking agents and initiators, a hydrophobic functional layer is formed. By rationally designing the ratio of reactants, the amount of fluorine and the length of fluorine chains are reduced, and uniform block copolymerization is achieved.

Benefits of technology

The prepared hydrophobic fabric has significant and efficient hydrophobic properties. The surface is grafted with a large number of double bonds to form an excellent hydrophobic functional layer. It is suitable for a variety of cellulose fabrics. The process is simple, non-toxic and harmless, and low in cost. It is applicable to outdoor sports equipment, marine rescue equipment, daily household products and medical protection.

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Abstract

The application relates to the technical field of new materials, and discloses a hydrophobic fabric and a preparation method and application thereof. The method comprises the following steps: (1) carrying out a first contact reaction on a fabric and a vinyl nitrogen heterocycle compound in the presence of a solvent, and obtaining a treated fabric I after washing; (2) adding an initiator and a crosslinking agent into the solvent to obtain a mixture I; (3) adding a fluorine-containing acrylic ester compound and an acrylamide compound into the mixture I to carry out a second contact reaction on the treated fabric I in an inert gas atmosphere, and obtaining a treated fabric II; and (4) rolling, baking and drying the treated fabric II in sequence to obtain a hydrophobic fabric. The method has the advantages of simple process flow, high efficiency and low cost, and the prepared hydrophobic fabric has excellent hydrophobic performance, self-cleaning ability and oil-water separation ability.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of new materials, in particular to a hydrophobic fabric and a preparation method and application thereof. BACKGROUND

[0002] As an important achievement of modern textile technology, hydrophobic fabric has become an indispensable material in many industries. This kind of textile product treated by special chemical process has unique self-cleaning, antibacterial, oil-water separation and other characteristics, and plays a crucial role in outdoor sports equipment, marine rescue equipment, daily household supplies and medical protection fields. With the development of society and the progress of science and technology, the demand for hydrophobic fabric is showing a rising trend.

[0003] However, the traditional hydrophobic fabric preparation technology has certain limitations. The acrylate hydrophobic agent widely used in the market can give the fabric hydrophobic properties to some extent, but its hydrophobic effect is relatively general, which is difficult to meet the application scenarios with higher performance requirements. On the other hand, although fluorine-based hydrophobic agents have superior hydrophobic properties, they often require the use of a large amount of fluorine atoms and long fluorine chains in the preparation process, which not only increases the production cost, but also may cause safety hazards to aquatic organisms due to the accumulation in the environment, which is not conducive to the sustainable development of the ecological environment.

[0004] In view of these problems, it is particularly important to research and develop a new type of hydrophobic fabric preparation technology. This technology should have the following characteristics: first, low fluorine content, reducing the potential impact on the environment; second, non-toxic and harmless, ensuring safety and reliability during use; third, simple process flow, facilitating large-scale industrial production; and finally, high efficiency and wide application range, which can shorten the production cycle and reduce costs while ensuring quality.

[0005] In summary, the research and promotion of this new type of hydrophobic fabric preparation technology is of great significance for promoting technological innovation and transformation and upgrading of the textile industry. Not only can it promote the green transformation of the textile industry and achieve sustainable development, but also can provide consumers with better and safer products. SUMMARY

[0006] The present application aims to overcome the technical problems of existing technology in the preparation of hydrophobic fabric, such as complex process, excessive introduction of fluorine atoms, long fluorine chain length, and the need to further improve the hydrophobic properties of the obtained hydrophobic fabric.

[0007] To achieve the above-mentioned purpose, the first aspect of the present application provides a method for preparing a hydrophobic fabric, which comprises the following steps:

[0008] (1) In the presence of a solvent, the fabric is subjected to a first contact reaction with a vinyl nitrogen heterocycle compound, and after washing, a treated fabric I is obtained;

[0009] (2) adding initiator and crosslinking agent into solvent to obtain mixture I;

[0010] (3) adding fluorine-containing acrylate compound and acrylamide compound into the mixture I to carry out second contact reaction to obtain treated fabric II in inert gas atmosphere; wherein the fluorine-containing acrylate compound and the acrylamide compound are added into the reaction system in three equal intervals, each interval is 20-40 min, and the weight ratio of the three times is 1:1:1-2;

[0011] (4) rolling, baking and drying the treated fabric II in sequence to obtain hydrophobic fabric;

[0012] The weight ratio of the total amount of the fluorine-containing acrylate compound to the amount of the initiator is 36-61:1.

[0013] The second aspect of the present application provides the hydrophobic fabric prepared by the method of the first aspect.

[0014] The third aspect of the present application provides the application of the hydrophobic fabric of the second aspect in manufacturing storm coat, life jacket, anti-fouling furniture or treating oil spill.

[0015] Compared with the prior art, the method provided by the present application has at least the following beneficial effects:

[0016] (1) The present application combines the hydrophobic advantages of acrylate and fluorine hydrophobic agent, reduces the amount of fluorine and the length of fluorine chain by reasonably designing the proportion of reaction substances and adding the fluorine-containing acrylate compound and the acrylamide compound in multiple times, avoids the disadvantages and hazards brought by using fluorine hydrophobic agent alone, realizes the uniform block copolymerization of the fluorine-containing acrylate compound and the acrylamide compound, and makes the structure of the polymer hydrophobic functional layer well constructed and the hydrophobic performance improved.

[0017] (2) The hydrophobic fabric prepared by the present application has significantly high hydrophobic performance, the nitrogen atom in the vinyl nitrogen heterocyclic compound and the oxygen atom on the fabric form ion-dipole interaction force, a large number of double bonds are grafted on the surface of the fabric to form a functionalized fabric. The fluorine-containing acrylate compound and the acrylamide compound are induced to initiate free radical copolymerization on the surface of the functionalized fabric by the initiator to form a hydrophobic functional layer. Among them, the fluorine atom has large electronegativity, small atomic radius, high bond energy of C-F bond and low surface tension, so that the fabric shows excellent hydrophobic effect.

[0018] (3) In the polymerization process, the crosslinking agent plays a role in regulating the molecular weight and molecular weight distribution, and the acrylamide compound avoids the steric hindrance effect of fluorine-containing acrylate compounds in the polymerization process, which is beneficial to the construction of the hydrophobic polymer functional layer.

[0019] (4) The hydrophobic fabric prepared by the application is suitable for immersion modification of most cellulose-containing fabrics, such as cotton fabric, cotton-polyester blended fabric, wool fabric, silk fabric and hemp fabric.

[0020] (5) The raw materials involved in the whole process of the hydrophobic fabric of the application are widely sourced and low in cost, and the preparation process is non-toxic and harmless compared with traditional acrylate and fluorine hydrophobic treatment, and has the advantages of simple process flow, high efficiency and good industrial application prospect. BRIEF DESCRIPTION OF DRAWINGS

[0021] Figure 1 is a real photo of the partially hydrophobic fabric prepared in the comparative example 3 and the comparative example 4 of the application;

[0022] Figure 2 is a water contact angle photo of the hydrophobic fabric prepared in the preferred embodiment of the application;

[0023] Figure 3 is a real photo of the hydrophobic fabric prepared in the comparative example 1 and the comparative example 2 of the application during water contact angle testing;

[0024] Figure 4 is an oil-water separation effect photo of the hydrophobic fabric prepared in the preferred embodiment of the application;

[0025] Figure 5 is a comparison photo of the self-cleaning effect of the hydrophobic fabric prepared in the preferred embodiment of the application;

[0026] Figure 6 is an underwater oil absorption effect photo of the hydrophobic fabric prepared in the preferred embodiment of the application;

[0027] Figure 7 is a real photo of the hydrophobic fabric prepared in the preferred embodiment of the application showing the "silver mirror phenomenon" in water;

[0028] Figure 8 is a real photo of the hydrophobic fabric prepared in the preferred embodiment of the application loaded with different stains;

[0029] Figure 9 is a real photo of the partially hydrophobic fabric prepared in the comparative example 5 of the application;

[0030] Figure 10 is a real photo of the partially hydrophobic fabric prepared in the comparative example 6 of the application. DETAILED DESCRIPTION

[0031] The endpoints of the ranges and any values disclosed herein are not limited to the precise values recited as the exact dimensions are not critical to the invention. Any numerical value, however, can include any values up to the stated range, value, or limit, and any value within the range, whether specifically disclosed or not. For ranges, the endpoints are included within the range.

[0032] The following terms are explained first in relation to the present invention.

[0033] In the present invention, the "vinyl nitrogen heterocycle compound" means an organic compound having a vinyl group and a ring structure containing at least one nitrogen atom, such as 4-vinylpyridine and 1-vinylimidazole.

[0034] The "fluorine-containing acrylate compound" means an organic compound having an acrylate group and at least one fluorine atom, such as hexafluorobutyl methacrylate and trifluoroethyl methacrylate.

[0035] The "acrylamide compound" means an organic compound having an acrylamide group, such as N,N-dimethylacrylamide and N-isopropylacrylamide.

[0036] As described above, the first aspect of the present invention provides a method for preparing a hydrophobic fabric, the method comprising the steps of:

[0037] (1) performing a first contact reaction of a fabric with a vinyl nitrogen heterocycle compound in the presence of a solvent, and obtaining a treated fabric I after rinsing;

[0038] (2) adding an initiator and a crosslinking agent to the solvent to obtain a mixture I;

[0039] (3) performing a second contact reaction of the treated fabric I with a fluorine-containing acrylate compound and an acrylamide compound in the mixture I in an inert gas atmosphere, to obtain a treated fabric II; wherein the fluorine-containing acrylate compound and the acrylamide compound are added to the reaction system in three equal intervals, each interval being 20-40 minutes, and the weight ratio of the amounts of the three times is 1:1:1-2, respectively;

[0040] (4) sequentially subjecting the treated fabric II to rolling, baking, and drying to obtain a hydrophobic fabric;

[0041] The weight ratio of the total amount of the fluorine-containing acrylate compound to the amount of the initiator is 36-61:1.

[0042] It should be noted that in the present application, the first part of the fluorine-containing acrylate compound, the second part of the fluorine-containing acrylate compound and the third part of the fluorine-containing acrylate compound together constitute the total amount of the fluorine-containing acrylate compound.

[0043] Similarly, it should be noted that in the present application, the first part of the acrylamide compound, the second part of the acrylamide compound and the third part of the acrylamide compound together constitute the total amount of the acrylamide compound.

[0044] Preferably, in step (1), the vinyl nitrogen heterocycle compound is selected from at least one of 4-vinylpyridine, 2-vinylpyridine, 1-vinylimidazole, 2-vinylpyrazine. This preferred case helps to form strong and stable chemical bonds on the surface of the fabric, form a uniform covering layer on the surface of the fabric, and significantly improve the hydrophobic performance, durability and comprehensive performance of the hydrophobic fabric.

[0045] Preferably, in step (1), the fabric is selected from at least one of polyester fabric, pure cotton fabric, hemp fabric, wool fabric.

[0046] Preferably, in step (1), the volume of the solvent used is not less than 20 times the weight of the fabric, wherein the volume of the solvent used is in mL and the weight of the fabric is in g.

[0047] Preferably, in steps (1) and (2), the solvent is toluene.

[0048] Preferably, in step (1), the flushing is performed using the solvent.

[0049] Preferably, in step (1), the weight ratio of the fabric to the vinyl nitrogen heterocycle compound is 1:2-11. This preferred case is more conducive to the full reaction of the vinyl nitrogen heterocycle compound with the fabric, so that the fabric surface is grafted with a large number of double bonds.

[0050] Preferably, in step (1), the first contact reaction is carried out under stirring conditions, and at least meets: temperature is 30-50℃, rotation speed is 250-400rpm, and time is 3h.

[0051] Preferably, in step (2), the initiator is selected from at least one of azobisisobutyronitrile, azobisisoheptyl nitrile, dimethyl azobisisobutyrate, benzoyl peroxide, tert-butyl peroxybenzoate, methyl ethyl ketone peroxide, tert-butyl peroxide, ammonium persulfate.

[0052] Preferably, in step (2), the crosslinking agent is N,N-methylenebisacrylamide and / or divinylbenzene.

[0053] Preferably, in step (3), the inert gas is nitrogen and / or argon.

[0054] Preferably, in step (3), the fluorine-containing acrylate compound is selected from at least one of hexafluorobutyl methacrylate, trifluoroethyl methacrylate, perfluoroalkyl ethyl methacrylate.

[0055] Preferably, in step (3), the acrylamide compound is selected from at least one of N,N-dimethyl acrylamide, N-isopropyl acrylamide, N-hydroxymethyl acrylamide, acrylamide.

[0056] According to a preferred embodiment, in step (3), the treated fabric I is added with the first part of fluorine-containing acrylate compound, the first part of acrylamide compound into the mixture I to start the second contact reaction, and this moment is recorded as t = 0; then the second part of fluorine-containing acrylate compound and the second part of acrylamide compound are continuously added at t = 30 min, the third part of fluorine-containing acrylate compound and the third part of acrylamide compound are continuously added at t = 60 min, and the second contact reaction is completed at t = 6-10 h.

[0057] Preferably, in step (3), the fluorine-containing acrylate compound and the acrylamide compound are added into the reaction system in three equal intervals, each interval being 20-40 min, and the weight ratio of the three times is 1:1:1. In this preferred case, it helps to improve the uniformity and grafting efficiency of the reaction, so that the hydrophobic fabric prepared has more excellent hydrophobic performance, stronger self-cleaning ability and higher oil-water separation efficiency.

[0058] Preferably, in step (3), the total weight of the amount of the fluorine-containing acrylate compound, the total weight of the amount of the acrylamide compound and the weight of the amount of the vinyl nitrogen heterocycle compound used in step (1) are in a ratio of 1-6:1:0.6-1.5.

[0059] More preferably, in step (3), the total weight of the amount of the fluorine-containing acrylate compound, the total weight of the amount of the acrylamide compound and the weight of the amount of the vinyl nitrogen heterocycle compound used in step (1) are in a ratio of 5-6:1:0.6-1.5.

[0060] Preferably, the weight ratio of the total amount of the fluorine-containing acrylate compound to the amount of the crosslinking agent is 15-30:1.

[0061] Preferably, in step (3), the conditions of the second contact reaction at least satisfy that the temperature is 50-75℃ and the rotation speed is 100-300rpm.

[0062] Preferably, in step (4), the conditions of the baking at least satisfy that the temperature is 130-140℃ and the time is 4min.

[0063] Preferably, in step (4), the temperature of the drying is 70℃.

[0064] As described above, the second aspect of the present application provides the hydrophobic fabric prepared by the method of the first aspect.

[0065] As described above, the third aspect of the present application provides the use of the hydrophobic fabric of the second aspect in manufacturing a storm coat, a life jacket, a stain-resistant furniture or treating an oil spill.

[0066] The present application is described in detail below by examples. The raw materials used in the examples are commercially available unless otherwise specified.

[0067] Fabric: pure cotton fabric;

[0068] Solvent: toluene;

[0069] Vinyl nitrogen heterocycle compound: 4-vinylpyridine;

[0070] Initiator: azobisisobutyronitrile;

[0071] Crosslinking agent: N,N-methylenebisacrylamide;

[0072] Fluorine-containing acrylate compound: hexafluorobutyl methacrylate;

[0073] Acrylamide compound: N,N-dimethylacrylamide.

[0074] Example 1

[0075] This example is used to illustrate the method for preparing the hydrophobic fabric provided by the present application, which is performed according to the following steps:

[0076] (1) 0.43g of the vinyl nitrogen heterocycle compound is added to 25mL of the solvent, and then the fabric is immersed in the mixture to perform the first contact reaction (the weight ratio of the fabric to the vinyl nitrogen heterocycle compound is 1:2), and then the fabric is taken out and washed with the solvent to obtain the treated fabric I;

[0077] The first contact reaction is performed under stirring, and the temperature is 45℃, the rotation speed is 350rpm, and the time is 3h.

[0078] (2) 0.045 g initiator and 0.085 g crosslinking agent were added to 40 mL solvent to obtain mixture I;

[0079] (3) The operation including the following steps was carried out under the conditions of nitrogen atmosphere, 70℃ and 170 rpm stirring:

[0080] The treated fabric I was added to the mixture I with the first part of fluorine-containing acrylate compounds and the first part of acrylamide compounds to start the second contact reaction, and the time was recorded as t = 0; then the second part of fluorine-containing acrylate compounds and the second part of acrylamide compounds were continuously added at t = 30 min, the third part of fluorine-containing acrylate compounds and the third part of acrylamide compounds were continuously added at t = 60 min, and the second contact reaction was completed at t = 8 h to obtain treated fabric II;

[0081] The weight ratio of the first part of fluorine-containing acrylate compounds, the second part of fluorine-containing acrylate compounds and the third part of fluorine-containing acrylate compounds is 1:1:1; the weight ratio of the first part of acrylamide compounds, the second part of acrylamide compounds and the third part of acrylamide compounds is 1:1:1;

[0082] The total weight of the fluorine-containing acrylate compounds is 2.29 g, and the total weight of the acrylamide compounds is 0.45 g;

[0083] (4) The treated fabric II was sequentially rolled, baked (temperature 135℃, time 4 min) and dried (temperature 70℃) to obtain a hydrophobic fabric, named P1.

[0084] Example 2

[0085] This example was carried out by a method similar to Example 1, except that in step (3), the total weight of the fluorine-containing acrylate compounds was 1.72 g;

[0086] Finally, a hydrophobic fabric was obtained, named P2.

[0087] Example 3

[0088] This example was carried out by a method similar to Example 1, except that in step (1), the amount of fabric was still 0.215 g, but the weight of the vinyl azacyclic compound was 0.24 g;

[0089] Finally, a hydrophobic fabric was obtained, named P3.

[0090] Example 4

[0091] This example was carried out using a similar method to Example 1, except that in step (3), the weight ratio of the first part of fluoroacrylate compound, the second part of fluoroacrylate compound and the third part of fluoroacrylate compound was 1:1:2; the weight ratio of the first part of acrylamide compound, the second part of acrylamide compound and the third part of acrylamide compound was 1:1:2.

[0092] Finally, a hydrophobic fabric was obtained, designated as P4.

[0093] Example 5

[0094] This example was carried out using a similar method to Example 1, except that in step (1), equal amounts of 2-vinylpyridine was used instead of 4-vinylpyridine.

[0095] Finally, a hydrophobic fabric was obtained, designated as P5.

[0096] Comparative Example 1

[0097] This comparative example was carried out using a similar method to Example 1, except that in step (3), the total amount of acrylamide compound was 0.

[0098] Finally, a hydrophobic fabric was obtained, designated as DP1.

[0099] Comparative Example 2

[0100] This comparative example was carried out using a similar method to Example 1, except that the operation in step (1) was not performed, specifically including:

[0101] S1, 0.045g initiator and 0.085g crosslinking agent were added to 40mL of solvent to obtain mixture I;

[0102] S2, the operation including the following steps was carried out under the conditions of nitrogen atmosphere, 70°C and 170rpm stirring:

[0103] 0.215g fabric was directly added to the first part of fluoroacrylate compound, the first part of acrylamide compound in the mixture I to start the second contact reaction, and the time was recorded as t=0; then the second part of fluoroacrylate compound and the second part of acrylamide compound were continuously added at t=30min, the third part of fluoroacrylate compound and the third part of acrylamide compound were continuously added at t=60min, and the second contact reaction was completed at t=8h to obtain treated fabric II;

[0104] The weight ratio of the first part of the fluorine-containing acrylate compound, the second part of the fluorine-containing acrylate compound and the third part of the fluorine-containing acrylate compound is 1:1:1; the weight ratio of the first part of the acrylamide compound, the second part of the acrylamide compound and the third part of the acrylamide compound is 1:1:1;

[0105] The total weight of the fluorine-containing acrylate compound is 2.29 g, and the total weight of the acrylamide compound is 0.45 g;

[0106] S3, the treated fabric II is sequentially rolled, baked (temperature is 135 DEG C, time is 4 min) and dried (temperature is 70 DEG C) to obtain a hydrophobic fabric, which is named as DP2.

[0107] Comparative Example 3

[0108] The present comparative example is carried out by using the similar method of Example 1, except that the operation in step (3) is different, which specifically comprises:

[0109] (3) under the conditions of nitrogen atmosphere, 70 DEG C and 170 rpm stirring, the treated fabric I is added into the mixture I with 2.29 g of the fluorine-containing acrylate compound and 0.45 g of the acrylamide compound at one time for the second contact reaction for 8 h to obtain a treated fabric II;

[0110] Finally, a hydrophobic fabric is obtained, which is named as DP3, Figure 1 Fig. (a) is a part of DP3, and the results show that the polymer functional layer on DP3 is too much, and the fabric surface appears to be polymerized, which causes the fabric to be unable to be normally used.

[0111] Comparative Example 4

[0112] The present comparative example is carried out by using the similar method of Example 1, except that in step (2), the weight of the initiator is increased to 0.077 g;

[0113] Finally, a hydrophobic fabric is obtained, which is named as DP4, Figure 1 Fig. (b) is a part of DP4, and the results show that the polymer functional layer on DP4 is too much, and the fabric surface appears to be polymerized, which causes the fabric to be unable to be normally used.

[0114] Comparative Example 5

[0115] The present comparative example is carried out by using the similar method of Example 1, except that in step (3), the fluorine-containing acrylate compound and the acrylamide compound are respectively divided into two times and added into the mixture I at t=0 and t=60 min, which specifically comprises:

[0116] (3) Perform the following operation under the conditions of nitrogen atmosphere, 70℃ and stirring at 170 rpm:

[0117] Add the treated fabric I and the first part of fluoroacrylate compound and the first part of acrylamide compound into the mixture I to start the second contact reaction, and mark this time as t = 0; then continue to add the second part of fluoroacrylate compound and the second part of acrylamide compound at t = 60 min, and complete the second contact reaction at t = 8h to obtain treated fabric II;

[0118] and the weight ratio of the use amount of the first part of fluoroacrylate compound to the second part of fluoroacrylate compound is 1:2, and the weight ratio of the use amount of the first part of acrylamide compound to the second part of acrylamide compound is 1:2;

[0119] Finally, a hydrophobic fabric is obtained, named DP5, Figure 9 which is a part of the actual picture of DP5, and the results show that the fabric surface of DP5 appears to have a polymerization explosion phenomenon, resulting in the fabric being unable to be normally used.

[0120] Comparative Example 6

[0121] This comparative example is performed by using a method similar to that of Example 1, except that in step (3), the weight ratio of the use amount of the first part of fluoroacrylate compound, the second part of fluoroacrylate compound and the third part of fluoroacrylate compound is 2:1:1; and the weight ratio of the use amount of the first part of acrylamide compound, the second part of acrylamide compound and the third part of acrylamide compound is 2:1:1;

[0122] Finally, a hydrophobic fabric is obtained, named DP6, Figure 10 which is a part of the actual picture of DP6, and the results show that the fabric surface of DP6 appears to have a polymerization explosion phenomenon, resulting in the fabric being unable to be normally used.

[0123] Test Example 1

[0124] Cut the hydrophobic fabric prepared as a sample to an appropriate size, and perform the following tests on the sample, and record part of the results in Table 1:

[0125] (1) Water contact angle and hydrophobic performance grade test:

[0126] According to the standard of GB / T 31906-2015;

[0127] (2) Oil-water separation efficiency test:

[0128] The filter device was used, with the sand core filter head as the joint, the 15 mL filter cup at the upper end, the 250 mL receiving bottle at the lower end, and the hydrophobic treated fabric as the separation medium placed on the sand core filter head and fixed with an aluminum alloy clamp. After mixing 4 mL of oil (chloroform, dyed with Sudan II) and 4 mL of water, the mixture was poured into the filter device. Due to the superhydrophobicity and superoleophilicity of the hydrophobic treated fabric, the oil could easily penetrate the fabric under the action of gravity, while the water was repelled at the upper end.

[0129] The oil-water separation efficiency η (%) was calculated by the following formula:

[0130]

[0131] wherein ma and mb are the weight of the collected water after separation and the mass of the original water in the oil-water mixture before separation, respectively.

[0132] (3) Self-cleaning ability test:

[0133] Prussian blue was used as the pollutant, and the Prussian blue powder was dispersed on the surface of the cut hydrophobic fabric and the original fabric (i.e. the pure cotton fabric used in Example 1), respectively, and then washed with clean water. If the Prussian blue powder on the surface of the hydrophobic treated fabric is washed away, and the surface of the product becomes clean and dry, it is recorded as strong self-cleaning ability of the hydrophobic fabric; if there is a small amount of Prussian blue powder remaining on the surface of the hydrophobic treated fabric, it is recorded as relatively strong self-cleaning ability; otherwise, it is recorded as weak self-cleaning ability.

[0134] (4) Underwater oil absorption ability test:

[0135] Red oil (chloroform, dyed) was added to the bottom of the beaker, and a piece of hydrophobic fabric was clamped with tweezers and immersed in water. If the oil is quickly absorbed after the hydrophobic fabric comes into contact with the oil, it is recorded as strong underwater oil absorption ability of the hydrophobic fabric; otherwise, it is recorded as weak underwater oil absorption ability.

[0136] (5) Silver mirror phenomenon test:

[0137] A piece of hydrophobic fabric was clamped with tweezers and immersed in water, and the silver mirror phenomenon (i.e. water cannot penetrate the surface of the hydrophobic fabric, and many bubbles are formed on the surface, which reflect and scatter light to some extent, making the surface look shiny, like a mirror) on the surface of the hydrophobic fabric in water was recorded.

[0138] Figure 2 Figures (a), (b), (c), and (d) show the water contact angle photos of P1, P2, P3, and P4, respectively;

[0139] Figure 3Fig. 1 (a) is a photograph of the water contact angle test of DP1, wherein the water droplet is dyed with methylene blue before being dropped onto the surface of the hydrophobic treated fabric, and the result shows that DP1 quickly absorbs water and does not have hydrophobic properties;

[0140] Figure 3 Fig. 1 (b) is a photograph of the water contact angle test of DP2, wherein the water droplet is dyed with methylene blue before being dropped onto the surface of the hydrophobic treated fabric, and the result shows that DP2 quickly absorbs water and does not have hydrophobic properties;

[0141] Figure 4 Fig. 2 shows the oil-water separation effect of P1, and the result shows that P1 has excellent oil-water separation capacity, and the oil-water separation efficiency reaches 99%;

[0142] Figure 5 Fig. 3 shows a comparison of the self-cleaning effect of the original fabric and P1, and the result shows that the surface of P1 is dry and clean without powder residue, and P1 has excellent self-cleaning capacity;

[0143] Figure 6 Fig. 4 shows the underwater oil absorption effect of P1, and the result shows that P1 has superhydrophobic and superoleophilic properties;

[0144] Figure 7 Fig. 5 shows a photograph of the "silver mirror phenomenon" of P1 in water, and the result shows that P1 has superhydrophobic properties;

[0145] Figure 8 Fig. 6 shows a photograph of P1 loaded with different stains, and the result shows that P1 has superhydrophobic stain removal properties.

[0146] Table 1

[0147]

[0148]

[0149] From the above results, it can be seen that the method provided by the present application involves a wide range of raw materials and low cost, and the whole process of the preparation process is simpler, more efficient, and has excellent hydrophobic properties, self-cleaning capacity and oil-water separation capacity compared with traditional hydrophobic treatment of acrylate and fluorine.

[0150] The above describes the preferred embodiments of the present application, but the present application is not limited thereto. Within the technical concept of the present application, various simple modifications can be made to the technical solutions of the present application, including the combination of various technical features in any other suitable manner, and these simple modifications and combinations should also be considered as disclosed by the present application and fall within the protection scope of the present application.

Claims

1. A method of making a hydrophobic fabric, characterized in that, The method comprises the following steps: (1) a first contact reaction of a fabric with a vinyl nitrogen heterocycle compound in the presence of a solvent, and after rinsing, a treated fabric I is obtained; (2) an initiator and a crosslinking agent are added to the solvent to obtain a mixture I; (3) in an inert gas atmosphere, the treated fabric I is added to the mixture I with a fluorine-containing acrylate compound and an acrylamide compound for a second contact reaction to obtain a treated fabric II; wherein the fluorine-containing acrylate compound and the acrylamide compound are added to the reaction system in three equal intervals, each interval being 20-40 min, and the weight ratio of the three times is 1:1:1-2; (4) the treated fabric II is sequentially rolled, baked and dried to obtain a hydrophobic fabric; The weight ratio of the total amount of the fluorine-containing acrylate compound to the amount of the initiator is 36-61:

1.

2. The method of claim 1, wherein, In step (1), the vinyl nitrogen heterocycle compound is selected from at least one of 4-vinylpyridine, 2-vinylpyridine, 1-vinylimidazole and 2-vinylpyrazine.

3. The method according to claim 1 or 2, characterized in that, In step (1), the weight ratio of the fabric to the vinyl nitrogen heterocycle compound is 1:2-11.

4. The method according to claim 1 or 2, characterized in that, In step (1), the first contact reaction is carried out under stirring, and at least meets the following conditions: temperature is 30-50℃, rotation speed is 250-400 rpm, and time is 3h.

5. The method according to claim 1 or 2, characterized in that, In step (3), the treated fabric I is added to the mixture I with a first part of the fluorine-containing acrylate compound and a first part of the acrylamide compound to start the second contact reaction, and the time is recorded as t=0; then a second part of the fluorine-containing acrylate compound and a second part of the acrylamide compound are continuously added at t=30min, a third part of the fluorine-containing acrylate compound and a third part of the acrylamide compound are continuously added at t=60min, and the second contact reaction is completed at t=6-10h.

6. The method of claim 1 or 2, wherein, In step (3), the fluorine-containing acrylate compound and the acrylamide compound are added to the reaction system in three equal intervals, each interval being 20-40 min, and the weight ratio of the three times is 1:1:

1.

7. The method according to claim 1 or 2, characterized in that, In step (3), the weight ratio of the total amount of the fluorine-containing acrylate compound, the total amount of the acrylamide compound to the amount of the vinyl nitrogen heterocycle compound used in step (1) is 1-6:1:0.6-1.

5.

8. The method of claim 1 or 2, wherein, In step (3), the second contact reaction at least meets the following conditions: temperature is 50-75℃, rotation speed is 100-300 rpm.

9. A hydrophobic fabric prepared by the method of any one of claims 1-8.

10. The use of the hydrophobic fabric of claim 9 in manufacturing a storm coat, a life jacket, a pollution-resistant furniture or treating an oil spill.

Citation Information

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