Oil-proof finishing agent for denim fabric and preparation method thereof

Abstract

The present invention provides a kind of denim fabric oil-proof finishing agent and preparation method thereof, the method comprising the following steps: (1) lauryl methacrylate, dodecafluoroheptyl methacrylate, butyl acrylate, sodium vinyl sulfonate are added to a reaction vessel, and then N, N-dimethylformamide and isopropylbenzene hydroperoxide are added to mix uniformly; (2) the system pH is adjusted to 8-12, and then butyl titanate and γ-aminopropyl triethoxysilane are added to react, and ultrapure water is added during the reaction, and the ultrasonic-microwave combined treatment system is fully dispersed, and then 2,2'-azo (2-methylpropyl amidine) is added dropwise to the reaction system to react. The oil-proof finishing agent prepared by the present invention integrates multiple functions, and not only has excellent oil and water repellency, but also has excellent antifouling property, water washing resistance and air permeability.

Description

Technical Field

[0001] The invention relates to the technical field of fabric finishing agents, and in particular to an oil-proof finishing agent for denim fabrics and a preparation method thereof. Background Art

[0002] Denim clothing is rugged, wear-resistant, comfortable and fashionable, and is favored by most people. However, denim clothing also has certain defects, such as poor oil and water repellency, easy to be stained with oil, and difficult to remove oil stains, and easy to be soaked in a humid environment, which reduces the beauty and comfort of denim clothing. Therefore, denim clothing needs to be oil-proof and water-repellent to make up for its shortcomings.

[0003] Oil-proof and water-repellent finishing means that the surface of the fabric after finishing has the performance of repelling oil and water liquid media, so as to achieve the effect of not affecting the comfort and breathability of the clothing, and effectively resisting the erosion of oil and water liquids to the human body. Currently, the commonly used oil-proof and water-repellent finishing agents mainly include quaternary ammonium compounds, paraffin-metal salts, resin derivatives, fatty acid aluminum, silicone, organic fluorine, etc. Among them, fluorine-containing water-repellent and oil-repellent finishing agents AG-480, finishing agent FG910, and finishing agent TG5541-A are more common. However, although the above-mentioned fluorine-containing water-repellent and oil-repellent finishing agents have better water-repellent and oil-repellent effects, the air permeability of the fabrics after finishing has decreased to varying degrees. Summary of the invention

[0004] In view of this, the present invention provides a method for preparing an oil-proof finishing agent for denim fabric, comprising the following steps:

[0005] (1) adding lauryl methacrylate, dodecafluoroheptyl methacrylate, butyl acrylate, and sodium vinyl sulfonate into a reaction container, and then adding N,N-dimethylformamide and cumene hydroperoxide in proportion, dispersing and mixing until uniform, to obtain a prepolymer for later use;

[0006] (2) The pH of the prepolymer system is adjusted to 8-12, and then a certain proportion of butyl titanate and γ-aminopropyltriethoxysilane are added to react, and a certain amount of ultrapure water is added during the reaction. Then, the prepolymer is placed in an ultrasonic-microwave combined treatment system for full dispersion, and then 2,2'-azo (2-methylpropylamidine) is added dropwise to the reaction system to react, thereby obtaining an oil-proof finishing agent for denim fabrics.

[0007] Furthermore, in step (1), the mass ratio of lauryl methacrylate, dodecafluoroheptyl methacrylate, butyl acrylate and sodium vinyl sulfonate is 3-6:3-6:1-2:2-3.

[0008] Furthermore, the amount of N,N-dimethylformamide added in step (1) accounts for 10%-30% of the total amount of monomers.

[0009] Furthermore, the amount of cumene hydroperoxide used in step (1) accounts for 0.1%-1.0% of the total amount of monomers.

[0010] Furthermore, the amount of butyl titanate added in step (2) accounts for 5%-10% of the total amount of monomers, and the mass ratio of γ-aminopropyltriethoxysilane to butyl titanate is 3-5:1-2.

[0011] Furthermore, the amount of 2,2'-azo(2-methylpropylamidine) used in step (2) accounts for 0.1%-0.5% of the total amount of monomers.

[0012] Furthermore, the reaction temperature in step (2) is 50-70° C., and the reaction time is 2-3 h.

[0013] Furthermore, in step (2), the power of the ultrasound is 30-100 W, the power of the microwave is 400-500 W, and the time of the ultrasound-microwave combined treatment is 10-20 min.

[0014] Furthermore, the amount of ultrapure water used in step (2) is 2-3 times the weight of the monomer.

[0015] The present invention also provides an oil-proof finishing agent for denim fabrics prepared according to the method.

[0016] Compared with the prior art, the present invention has the following beneficial effects: the oil-proof finishing agent prepared by the present invention integrates multiple functions in one, and not only has the characteristics of oil and water repellency, but also has multiple functions such as excellent anti-fouling property, water washability and air permeability, thereby solving the defect that the existing oil-proof finishing agent for fabrics has a single function and cannot meet people's different needs. DETAILED DESCRIPTION

[0017] In order to make the purpose, technical solution and advantages of the present invention clearer, the technical solution of the present invention will be described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work belong to the scope of protection of the present invention.

[0018] The experimental methods or test methods described in the following examples are conventional methods unless otherwise specified; the raw materials and auxiliary agents are obtained from conventional commercial channels or prepared by conventional methods unless otherwise specified.

[0019] Example 1

[0020] A method for preparing an oil-proof finishing agent for denim fabrics, the specific steps are as follows:

[0021] (1) adding lauryl methacrylate, dodecafluoroheptyl methacrylate, butyl acrylate, and sodium vinyl sulfonate monomer raw materials into a beaker at a mass ratio of 3:3:1:2, and then adding 10% of the total mass of N,N-dimethylformamide and 10% of the total mass of isopropylbenzene hydroperoxide, stirring until the mixture is uniform, and reacting at 55° C. for 20 minutes to obtain a prepolymer for standby use;

[0022] (2) The pH of the prepolymer is adjusted to 8, and then butyl titanate and γ-aminopropyl triethoxysilane are added to react, wherein the amount of butyl titanate added accounts for 5% of the total mass of the monomers, and the mass ratio of γ-aminopropyl triethoxysilane to butyl titanate is 3:1. Then, ultrapure water twice the total mass of the monomers is added to the reaction system, and then the system is placed in an ultrasonic-microwave combined treatment system for full dispersion, wherein the power of the ultrasonic wave is 30 W, the power of the microwave is 400 W, and the ultrasonic-microwave combined treatment time is 10 min. 2,2'-azo (2-methylpropyl amidine) is added dropwise to the reaction system, wherein the amount of 2,2'-azo (2-methylpropyl amidine) accounts for 0.1% of the total amount of the monomers, and a reaction is carried out to obtain an oil-proof finishing agent for denim fabrics.

[0023] Example 2

[0024] A method for preparing an oil-proof finishing agent for denim fabrics, the specific steps are as follows:

[0025] (1) adding lauryl methacrylate, dodecafluoroheptyl methacrylate, butyl acrylate, and sodium vinyl sulfonate monomer raw materials into a beaker in a mass ratio of 4:5:2:3, and then adding 20% ​​of the total mass of N,N-dimethylformamide and 20% of the total mass of isopropylbenzene hydroperoxide, stirring until the mixture is uniform, and reacting at 55° C. for 20 minutes to obtain a prepolymer for standby use;

[0026] (2) The pH of the prepolymer system is adjusted to 10, and then butyl titanate and γ-aminopropyl triethoxysilane are added to react, wherein the amount of butyl titanate added is 8% of the total mass of the monomers, and the mass ratio of γ-aminopropyl triethoxysilane to butyl titanate is 4:1. Then, ultrapure water 3 times the total mass of the monomers is added to the reaction system, and then the system is placed in an ultrasonic-microwave combined treatment system for full dispersion, wherein the power of the ultrasonic wave is 80 W, the power of the microwave is 450 W, and the ultrasonic-microwave combined treatment time is 15 min. 2,2'-azo (2-methylpropyl amidine) is added dropwise to the reaction system, wherein the amount of 2,2'-azo (2-methylpropyl amidine) is 0.2% of the total amount of the monomers, and a reaction is carried out to obtain an oil-proof finishing agent for denim fabrics.

[0027] Example 3

[0028] A method for preparing an oil-proof finishing agent for denim fabrics, the specific steps are as follows:

[0029] (1) adding lauryl methacrylate, dodecafluoroheptyl methacrylate, butyl acrylate, and sodium vinyl sulfonate monomer raw materials into a beaker at a mass ratio of 6:6:2:3, and then adding 30% of the total mass of N,N-dimethylformamide and 30% of the total mass of isopropylbenzene hydroperoxide, stirring until the mixture is uniform, and reacting at 55° C. for 20 minutes to obtain a prepolymer for standby use;

[0030] (2) The pH of the prepolymer system is adjusted to 12, and then butyl titanate and γ-aminopropyl triethoxysilane are added to react, wherein the amount of butyl titanate added accounts for 10% of the total mass of the monomers, and the mass ratio of the γ-aminopropyl triethoxysilane to butyl titanate is 5:2. Then, ultrapure water 3 times the total mass of the monomers is added to the reaction system, and then the system is placed in an ultrasonic-microwave combined treatment system for full dispersion, wherein the power of the ultrasonic wave is 100 W, the power of the microwave is 500 W, and the ultrasonic-microwave combined treatment time is 20 min. 2,2'-azo (2-methylpropyl amidine) is added dropwise to the reaction system, wherein the amount of the 2,2'-azo (2-methylpropyl amidine) accounts for 0.5% of the total amount of the monomers, and a reaction is carried out to obtain an oil-proof finishing agent for denim fabrics.

[0031] Comparative Example 1

[0032] A method for preparing an oil-proof finishing agent for denim fabrics, which differs from Example 1 in that γ-aminopropyltriethoxysilane is replaced by KH570.

[0033] Comparative Example 2

[0034] A method for preparing an oil-proof finishing agent for denim fabrics, which differs from Example 1 in that an ultrasonic-microwave combined processing system is not used for dispersion.

[0035] Comparative Example 3

[0036] A method for preparing an oil-proof finishing agent for denim fabrics, which is different from Example 1 in that the mass ratio of lauryl methacrylate, dodecafluoroheptyl methacrylate, butyl acrylate and sodium vinyl sulfonate is 7:7:3:5.

[0037] Comparative Example 4

[0038] A method for preparing an oil-proof finishing agent for denim fabrics, which is different from Example 1 in that the mass ratio of lauryl methacrylate, dodecafluoroheptyl methacrylate, butyl acrylate and sodium vinyl sulfonate is 2:2:0.5:1.

[0039] The performance of the oil-proof finishing agents prepared in Examples 1-3 and Comparative Examples 1-4 was tested. The pretreatment of denim fabrics, performance testing methods and test results are as follows.

[0040] (1) The selected denim fabric is pure cotton indigo dyed denim fabric provided by Guangdong Jun'an Denim Garment Research Institute. The denim fabric is desized in advance, and then the desized denim fabric is immersed in an oil-proof finishing agent.

[0041] (2) Detection method:

[0042] Water repellency: According to the AATCC-22-2005 "Water Repellency Test Spray Method", the test is conducted on a fabric water stickiness meter and scored using a standard wetting card. According to the requirements of American clothing retail companies for pure cotton products, the score must be 90 points before washing, 90 points after 3 washes, and 70 points after 30 washes to be qualified.

[0043] Oil repellency, tested according to AATCC-118-2007 standard, 8 is the best, 1 is the worst, the original oil repellency reaches 5, after 3 times of water washing, it reaches 4, and after 30 times of water washing, it reaches 3 for passing;

[0044] Washing resistance: the finished samples were tested on a SW-12 washing fastness tester. The finished fabrics were washed and dried, and then their oil and water repellency were measured.

[0045] Air permeability: cut a 20cm×20cm piece of denim fabric and test it on an air permeability tester.

[0046] (3) The test results are shown in Table 1.

[0047] Table 1

[0048]

[0049] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A method for preparing an oil-proof finishing agent for denim fabric, characterized in that: The following steps are involved: (1) Lauryl methacrylate, dodecafluoroheptyl methacrylate, butyl acrylate, and sodium vinyl sulfonate are added to a reaction container, and then N,N-dimethylformamide and cumene hydroperoxide are added in proportion, and the mixture is dispersed until uniformly mixed to obtain a prepolymer for use; (2) The pH of the prepolymer system is adjusted to 8-12, and then a certain proportion of butyl titanate and γ-aminopropyltriethoxysilane are added to react, and a certain amount of ultrapure water is added during the reaction, and then placed in an ultrasonic-microwave combined treatment system for full dispersion, and then 2,2'-azo (2-methylpropylamidine) is added dropwise to the reaction system to react, thereby obtaining an oil-proof finishing agent for denim fabrics; In step (1), the mass ratio of lauryl methacrylate, dodecafluoroheptyl methacrylate, butyl acrylate and sodium vinyl sulfonate is 3-6:3-6:1-2:2-3.

2. The method for preparing the oil-proof finishing agent for denim fabric according to claim 1, characterized in that: The amount of N,N-dimethylformamide added in step (1) accounts for 10%-30% of the total amount of monomers.

3. The method for preparing the oil-proof finishing agent for denim fabric according to claim 1, characterized in that: The amount of cumene hydroperoxide used in step (1) is 0.1%-1.0% of the total amount of monomers.

4. The method for preparing the oil-proof finishing agent for denim fabric according to claim 1, characterized in that: In step (2), the amount of butyl titanate added is 5%-10% of the total amount of monomers, and the mass ratio of γ-aminopropyltriethoxysilane to butyl titanate is 3-5:1-2.

5. The method for preparing the oil-proof finishing agent for denim fabric according to claim 1, characterized in that: The amount of 2,2'-azo(2-methylpropylamidine) used in step (2) accounts for 0.1-0.5% of the total amount of monomers.

6. The method for preparing the oil-proof finishing agent for denim fabric according to claim 1, characterized in that: The reaction temperature in step (2) is 50-70°C and the reaction time is 2-3h.

7. The method for preparing the oil-proof finishing agent for denim fabric according to claim 1, characterized in that: In step (2), the power of the ultrasound is 30-100 W, the power of the microwave is 400-500 W, and the time of the ultrasound-microwave combined treatment is 10-20 min.

8. The method for preparing the oil-proof finishing agent for denim fabric according to claim 1, characterized in that: The amount of ultrapure water used in step (2) is 2-3 times the weight of the monomer.

9. An oil-proof finishing agent for denim fabrics prepared by the method according to any one of claims 1 to 8.

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