A kind of jacket repairing agent and preparation method thereof

Abstract

The present invention relates to a kind of jacket repair agent and preparation method thereof, the jacket repair agent comprises the following components by mass fraction: gelatin-acrylate-siloxane copolymer 1-5%, aminosiloxane 5-20%, cationic surfactant 0.5-2%, auxiliary agent 1-5%, solvent remainder; wherein the gelatin-acrylate-siloxane copolymer is obtained by polymerization of acrylate-based gelatin, acryloxy polysiloxane and alkyl acrylate. The jacket repair agent of the present invention effectively improves adhesion and enhances the protection effect against water, spraying it on the surface of the jacket can achieve strong waterproof performance, and at the same time, it is easy to use, safe in ingredients, and has good application prospects.

Description

Technical Field

[0001] The invention relates to the technical field of clothing washing and care, in particular to a jacket repairing agent and a preparation method thereof. Background Art

[0002] As a key equipment for outdoor sports, the main functions of a jacket include windproof, waterproof and wear-resistant, so as to protect outdoor athletes from the influence of adverse weather and environment.

[0003] The material of the jacket is of great significance in terms of waterproof performance. The company's GORE-TEX microporous fabric is one of the most representative materials. GORE-TEX fabric is made of polytetrafluoroethylene that is quickly stretched and heated to form an expanded polytetrafluoroethylene microporous structure. This fabric is usually located in the middle layer of the laminated fabric, providing the jacket with excellent waterproof performance. Although waterproof fabrics such as GORE-TEX perform well in terms of waterproof performance, there are still problems with the outer layer of the jacket. Regardless of whether the outer layer is natural fiber or chemical fiber, it will be soaked when it comes into contact with water. After the entire garment is soaked, the breathability drops sharply. At this time, compared with traditional raincoats, the jacket has lost its obvious advantage.

[0004] To solve this problem, jackets usually need to undergo surface water-repellent treatment and heat curing. However, water-repellent treatment is not permanently effective, and the jacket will lose its effect after daily wear or rain and snow. Common surface water-repellent treatment methods include the use of fluorocarbons (such as perfluorooctanoic acid). However, fluorides are difficult to degrade and may cause lasting damage to the body through bioaccumulation. Therefore, more and more products are required to be fluorocarbon-free (PFC free).

[0005] In summary, there is an urgent need to develop a new technical solution and a new waterproofing solution that does not contain fluorocarbons to solve the problems existing in the existing technology and meet the market and consumer needs. Summary of the invention

[0006] Based on this, the present invention provides a jacket repair agent and a preparation method thereof. The jacket repair agent provided by the present invention uses gelatin, acrylate and siloxane as raw materials to prepare a copolymer, which is then compounded with aminosiloxane and other ingredients to effectively improve the adhesion and enhance the water protection effect. Spraying it on the surface of the jacket can achieve strong waterproof performance. At the same time, it is easy to use and has safe ingredients, and has good application prospects.

[0007] One object of the present invention is to provide a jacket repair agent, which comprises the following components in mass fraction:

[0008]

[0009]

[0010] in,

[0011] The gelatin-acrylate-siloxane copolymer is obtained by polymerizing acrylate-based gelatin, acryloxy polysiloxane and alkyl acrylate.

[0012] Furthermore, in the gelatin-acrylate-siloxane copolymer, the mass ratio of acrylate-based gelatin, acryloxypolysiloxane and alkyl acrylate is 1:(1-5):(0.5-2).

[0013] Furthermore, the alkyl group in the alkyl acrylate is selected from a C4-C20 straight-chain alkyl group.

[0014] Furthermore, the aminosiloxane is a siloxane having a quaternary ammonium salt group.

[0015] Furthermore, the cationic surfactant is preferably alkyl dimethyl polyoxyethylene ammonium chloride.

[0016] Furthermore, the auxiliary agent is selected from one or more of inorganic salts, cosolvents, fluorescent whitening agents, regulators, preservatives, colorants, color stabilizers and liquid flavors.

[0017] Another object of the present invention is to provide a method for preparing the above-mentioned jacket repair agent, the method for preparing the jacket repair agent comprising the following steps:

[0018] S1, mixing gelatin and acrylic anhydride, heating and reacting to obtain acrylate-based gelatin;

[0019] S2, mixing the acrylate-based gelatin, acryloxy polysiloxane and initiator, and heating them under the protection of inert gas to react, to obtain an intermediate product;

[0020] S3, adding alkyl acrylate to the intermediate product, heating and reacting, to obtain a gelatin-acrylate-siloxane copolymer;

[0021] S4. Mix the gelatin-acrylate-siloxane copolymer with other ingredients, stir evenly, and obtain a jacket repair agent.

[0022] Furthermore, in step S1, the temperature of the heating reaction is 30-60°C.

[0023] Furthermore, in step S2, the temperature of the heating reaction is 50-70°C.

[0024] Furthermore, in step S3, the temperature of the heating reaction is 60-80°C.

[0025] The present invention has the following beneficial effects:

[0026] In the raincoat repair agent provided by the present invention, materials such as gelatin-acrylate-siloxane copolymer, aminosiloxane, and cationic surfactant are compounded. Among them, the gelatin-acrylate-siloxane copolymer first reacts gelatin with acrylic anhydride to introduce acrylate groups, and then undergoes free radical polymerization with acryloxypolysiloxane and alkyl acrylate to obtain a product containing hydrophilic gelatin segments, as well as hydrophobic polydimethylsiloxane and fatty acid long-chain structures. The gelatin has a large number of polar groups and good adhesion, thereby improving the adhesion stability on the surface of the raincoat, and the hydrophobic segments are entangled with each other to form a network structure, giving the raincoat good waterproofness. At the same time, the introduced siloxane segments have good flexibility, which also ensures that the raincoat fabric is softer and skin-friendly. In addition, the aminosilicone and alkyl dimethyl polyoxyethylene ammonium chloride added in the present invention contain hydrophilic cationic quaternary ammonium salt structures and hydrophobic structures such as siloxane and alkyl chains, which not only have good compatibility with gelatin-acrylate-silicone copolymers, but also can play a role in auxiliary dispersion and stabilization, improve the stability of the product under various storage conditions, and can also synergistically enhance the water resistance of the jacket, and achieve the effects of splash-proof and bubble-proof. In summary, the jacket repair agent of the present invention does not contain fluorocarbon compounds, and can achieve excellent waterproof performance, overcome the deficiencies in the prior art, and has good application prospects. DETAILED DESCRIPTION

[0027] In order to more clearly illustrate the technical solution of the present invention, the following examples are listed. Unless otherwise stated, the raw materials, reactions and post-treatment methods shown in the examples are common raw materials on the market and technical methods well known to those skilled in the art.

[0028] The words "preferred", "preferably", "more preferably", etc. in the present invention refer to embodiments of the present invention that can provide certain beneficial effects in certain circumstances. However, other embodiments may also be preferred under the same circumstances or other circumstances. In addition, the description of one or more preferred embodiments does not imply that other embodiments are not applicable, nor is it intended to exclude other embodiments from the scope of the present invention.

[0029] It should be understood that, except in any operating examples, or where otherwise indicated, all numbers indicating, for example, the amounts of ingredients used in the specification and claims should be understood to be modified in all cases by the term "about". Therefore, unless indicated to the contrary, the numerical parameters set forth in the following specification and the appended claims are approximate values ​​that vary depending on the desired properties to be obtained by the present invention.

[0030] The aminosilicone in the embodiment of the present invention is a polysiloxane having a diquaternary ammonium salt group, purchased from Innocare Company with the brand name Innocare QSQ01.

[0031] The cationic surfactant in the embodiment of the present invention is alkyl dimethyl polyoxyethylene ammonium chloride, purchased from Innocare Company with the brand name Innocare HEX25.

[0032] The preservative in the embodiment of the present invention is kason, purchased from Clariant, model number Nipaguard CG.

[0033] The gelatin in the examples of the present invention was purchased from Guangzhou Huayu Biotechnology Co., Ltd.

[0034] The methacryloxypropyl di-terminated polydimethylsiloxane in the embodiment of the present invention is purchased from Aladdin, and has a molecular weight of 8000-12000.

[0035] The components and mass fractions of the jacket repair agents of Examples 1-3 are shown in Table 1.

[0036] Table 1 Composition and mass fraction of Examples 1-3

[0037]

[0038]

[0039] The preparation method of the jacket repair agent of Examples 1-3 comprises the following steps:

[0040] S1. Use water as solvent, add gelatin and stir for 0.5h, adjust pH to 7.5 with 2mol / L NaOH solution, then add methacrylic anhydride (gelatin: methacrylic anhydride = 1:0.9, m / m), react at 50°C for 3h, dialyze for 3 days (KDa = 10000), and freeze-dry to obtain acrylate-based gelatin;

[0041] S2, using water as solvent, mixing the acrylate-based gelatin, methacryloyloxypropyl di-terminated polydimethylsiloxane, and potassium persulfate in a mass ratio of 1:1.5:0.05, and reacting at 60° C. for 2 h under nitrogen protection to obtain an intermediate product;

[0042] S3, adding lauryl acrylate to the intermediate product (acrylate-based gelatin: lauryl acrylate=1:0.8, m / m), reacting at 65° C. for 2 h, removing the solvent, and drying to obtain a gelatin-acrylate-siloxane copolymer;

[0043] S4. According to the above mass fractions, the gelatin-acrylate-siloxane copolymer is mixed with other ingredients, and stirred evenly to obtain a jacket repair agent.

[0044] Comparative Examples 1-2 were set based on the examples.

[0045] The difference between Comparative Example 1 and Example 1 is that step S3 is omitted, the product of step S2 is dried and replaced with gelatin-acrylate-siloxane copolymer of equal mass, and the other ingredients and preparation method are the same as those of Example 1.

[0046] The difference between Comparative Example 2 and Example 1 is that the aminosilicone is replaced by an aminosilicone oil of equal mass (Jinan Silicon Port Chemical Co., Ltd., brand 03), and the other ingredients and preparation method are the same as those of Example 1.

[0047] Test Example 1

[0048] The stability test was performed on Examples 1-3 and Comparative Examples 1-2.

[0049] Test method:

[0050] Low temperature stability test: After the jacket repair agent is bottled and sealed, it is placed in an environment with a temperature of 0±2℃. After being kept at a constant temperature for 2 months, it is taken out and restored to room temperature to observe the appearance. If the sample has no obvious color change, stratification or precipitation, it is judged to be qualified for low temperature stability.

[0051] Test of room temperature stability: After the jacket repair agent is bottled and sealed, it is placed in an environment with a temperature of 25±2℃. After being placed at a constant temperature for 2 months, it is taken out and the appearance is immediately observed. If there is no obvious discoloration, stratification or precipitation of the sample, it is judged to be qualified for room temperature stability.

[0052] High temperature stability test: After the jacket repair agent is bottled and sealed, it is placed in an environment with a temperature of 45±2℃. After being kept at a constant temperature for 2 months, it is taken out and restored to room temperature to observe the appearance. If the sample has no obvious color change, stratification or precipitation, it is judged to be qualified for high temperature stability.

[0053] The test results are shown in Table 2.

[0054] Table 2 Stability test results

[0055] project Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 High temperature stability qualified qualified qualified Failure qualified Room temperature stability qualified qualified qualified qualified qualified Low temperature stability qualified qualified qualified Failure Failure

[0056] According to Table 2, the samples prepared in Examples 1-3 did not change color, delaminate or precipitate after being placed at different temperatures for two months, which proves that the components of the composition have good compatibility and strong product stability. In Comparative Example 1, the modified component did not introduce a long alkyl chain, and the stability was reduced, and turbidity and stratification occurred under high and low temperature environments. In Comparative Example 2, aminosilicone was replaced with aminosilicone oil, which was unstable at low temperatures and easily led to gelation and turbidity and stratification.

[0057] Test Example 2

[0058] The waterproof properties of Examples 1-3 and Comparative Examples 1-2 were tested.

[0059] Test method:

[0060] (1) Preparation of test equipment:

[0061] The water spraying device consists of a vertically clamped 150mm funnel and a metal nozzle, where the distance from the top of the funnel to the bottom of the nozzle is 190-200mm, and a 10mm diameter rubber hose is used to connect the nozzle and the funnel. The metal nozzle needs to have a convex circular surface with evenly distributed spray holes, and 250ml of water is injected into it for a continuous spraying time of 25-30s. The sample holder consists of two wooden or metal rings that can cooperate with each other, and the sample needs to be tightly clamped in it. During the test, the clamp ring needs to be placed on a suitable pillar at a 45° inclination, and the center of the test surface is 150mm below the center of the nozzle surface.

[0062] (2) Test steps:

[0063] The same model of jackets were sprayed with the jacket repair agent prepared in the embodiment or the comparative example, and then 3 pieces of 180 mm2 of the area were taken from different parts of each jacket. 2 As a specimen, try to avoid touching it with your hands after sampling. The specimen should be as representative as possible and avoid taking any creases.

[0064] After taking the sample, it needs to be placed at room temperature for 24 hours of humidity conditioning. After humidity conditioning, clamp the sample with a sample holder and place it on a support. During the test, the fabric side should face upwards. Unless otherwise required, the warp direction of the sample should be parallel to the water flow direction.

[0065] Quickly and steadily inject 250ml (20±2℃) distilled water into the funnel so that the watering continues. Once the watering stops, quickly remove the holder together with the sample, make the fabric face downward horizontally, and then gently tap it twice against a hard object (once at two opposite points in the radial direction). After the tapping, the sample is still in the holder, and its grade is evaluated according to the observed wetness of the sample.

[0066] Water level:

[0067] Level 1: The exposed surface is completely wetted;

[0068] Level 2: Half of the showered surface is wetted, usually referring to the sum of the wetted areas of small unconnected patches;

[0069] Level 3: Only a small, unconnected area of ​​the showered surface is wetted;

[0070] Level 4: The showered surface is not wet, but there are small water droplets on the surface;

[0071] Level 5: The surface is not wet and there are no water droplets on the surface.

[0072] The test results are shown in Table 3.

[0073] Table 3 Waterproof test results

[0074] project Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 The first specimen 5 5 4 3 3 The second sample 4 5 5 3 4 The third specimen 5 5 5 4 4 Average grade 4.7 5 4.7 3.3 3.7

[0075] According to Table 3, compared with Comparative Example 1-2, the added gelatin-acrylate-siloxane copolymer and aminosiloxane in Example 1-3 can play a synergistic role, giving the jacket good waterproof properties. The waterproof performance of Comparative Example 1-2 with changed components is not ideal. In summary, the present invention overcomes the defects existing in the prior art and has good application prospects.

[0076] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the present invention can be implemented in other specific forms without departing from the spirit or essential features of the present invention. Therefore, the embodiments should be considered exemplary and non-restrictive in all respects, and the scope of the present invention is defined by the appended claims rather than the above description, and it is intended that all changes falling within the meaning and scope of the equivalent elements of the claims be included in the present invention.

[0077] In addition, it should be understood that although the present specification is described according to implementation modes, not every implementation mode contains only one independent technical solution. This description of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment may also be appropriately combined to form other implementation modes that can be understood by those skilled in the art.

Claims

1. A jacket repair agent, characterized in that: The jacket repair agent includes the following components by mass fraction: Gelatin-acrylate-siloxane copolymer 1-5% Aminosiloxane 5-20% Cationic surfactant 0.5-2% Additives 1-5% Solvent residue; in, The gelatin-acrylate-siloxane copolymer is obtained by polymerization of acrylate-based gelatin, acryloxy polysiloxane and alkyl acrylate; In the gelatin-acrylate-siloxane copolymer, the mass ratio of acrylate-based gelatin, acryloxypolysiloxane and alkyl acrylate is 1:(1-5):(0.5-2); The alkyl group in the alkyl acrylate is selected from a C4-C20 straight chain alkyl group; The aminosilicone is a siloxane having a quaternary ammonium salt group; The preparation method of the jacket repair agent comprises the following steps: S1, mixing gelatin and acrylic anhydride, heating and reacting to obtain acrylate-based gelatin; S2, mixing the acrylate-based gelatin, acryloxy polysiloxane and initiator, and heating them under the protection of inert gas to react, to obtain an intermediate product; S3, adding alkyl acrylate to the intermediate product, heating and reacting, to obtain a gelatin-acrylate-siloxane copolymer; S4, mixing the gelatin-acrylate-siloxane copolymer with other ingredients, stirring evenly, to obtain a jacket repair agent; The acryloxy polysiloxane is methacryloxypropyl double-terminated polydimethylsiloxane.

2. The jacket repair agent according to claim 1, characterized in that: The auxiliary agent is selected from one or more of inorganic salts, cosolvents, fluorescent whitening agents, preservatives, colorants, color stabilizers and liquid flavors.

3. The jacket repair agent according to claim 1, characterized in that: In step S1, the temperature of the heating reaction is 30-60°C.

4. The jacket repair agent according to claim 1, characterized in that: In step S2, the temperature of the heating reaction is 50-70°C.

5. The jacket repair agent according to claim 1, characterized in that: In step S3, the temperature of the heating reaction is 60-80°C.

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