Finishing agent for bone feeling style finishing as well as preparation method and application of finishing agent

The prepared skin-like finishing agent solves the problems of poor stability and excessive formaldehyde in the existing technology, and realizes the softness and hardness of the fabric, which is both soft and hard, and simplifies the Use process.

CN119162828APending Publication Date: 2024-12-20HANGZHOU TRANSFAR FINE CHEM CO LTD +2
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Patent Information

Application Number
CN202411415324.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-11
Publication Date
2024-12-20

AI Technical Summary

Technical Problem

The existing skin-like finishing agent has poor stability in terms of soft feel and hard rigidity. It requires on-site compounding of hard rigidity and silicone oil. The process is complicated and there is a problem of excessive formaldehyde and hard rigidity easily disappearing.

Method used

The emulsion polymerization reaction is carried out under the combined action of crosslinking agent, buffering agent, emulsifier and initiator, and the emulsifier is added later in the reaction. Silicone oil, prepared finishing agent.

Benefits of technology

This finishing agent does not contain formaldehyde and has good stability. It can combine excellent toughness, soft feel and suitable stiffness and rigidity, meeting the skinny style requirements. Users do not need to temporarily add silicone oil to simplify the process to avoid the problem of excessive formaldehyde and rigidity disappearance of rigidity. .

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Abstract

The invention belongs to the technical field of textile style finishing, and particularly relates to a finishing agent for bone feeling style finishing and a preparation method and application thereof. The finishing agent provided by the invention is prepared by taking a vinyl acetate monomer, polyvinyl alcohol, acrylate and a polyfunctional acrylic monomer as raw materials, carrying out emulsion polymerization reaction under the combined action of a cross-linking agent, a buffer agent, an emulsifier and an initiator, and adding block silicone oil at the later stage of the reaction. The finishing agent does not contain formaldehyde and is good in stability, and a fabric finished by the finishing agent can have excellent toughness, soft hand feeling and proper stiffness and rigidity, and meets the requirements of customers on bone feeling styles.
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Description

Technical Field

[0001] The present application belongs to the technical field of textile style finishing, and more specifically, relates to a finishing agent for skinny style finishing, a preparation method and application thereof. Background Art

[0002] As an important finishing method for textiles, bone-feeling finishing requires the finished fabric to have a soft hand feel and stiffness, referred to as bone-feeling. It is widely used in the finishing of Roman cloth, cotton twill and other clothing fabrics. At present, bone-feeling finishing is mainly achieved by using stiffeners on-site with softeners. There are two main types of stiffeners used, one is melamine resin containing formaldehyde, and the other is white latex (polyvinyl acetate).

[0003] Melamine resin and silicone oil are usually used as finishing agents for skinny style finishing. Although stiffness and softness are mutually exclusive, melamine resin can play a role of cross-linking, and the cross-linking is sufficient, which can become the skeleton after skinny style finishing, so that the stiff effect produced by it can still maintain the stiff style when silicone oil plays a softening role, so that the finished fabric has an excellent skinny effect. However, melamine formaldehyde resin itself contains a large amount of formaldehyde, which makes the formaldehyde on the surface of the finished fabric exceed the standard, affecting the quality of the finished fabric and seriously endangering the physical and mental health of producers and users. In addition, the pH value of silicone oil is acidic, and melamine resin is easy to catalyze cross-linking under acidic conditions. Therefore, the finishing agent needs to compound and adjust the stiffening agent (melamine resin) and silicone oil on site, making the skinny style finishing process complicated.

[0004] White latex does not contain formaldehyde and can adhere to the surface of fabrics by forming a film, thus giving the fabric a stiff and rigid effect. It can replace melamine resin and silicone oil for compounding as a skinny style finishing agent. However, white latex does not produce a cross-linking effect, and the stiff style it produces is easily affected by the softening effect of silicone oil, resulting in insufficient stiffness of the finishing agent. When the finished fabric is kneaded many times, the stiff and rigid style disappears. Since the stiff style produced by white latex is not significant and is easily affected by silicone oil, it is necessary to adjust the amount of white latex and silicone oil on site to achieve skinny style finishing. Summary of the invention

[0005] In view of the defects of the prior art, the purpose of this application is to provide a finishing agent for bone-feeling style finishing, its preparation method and application, aiming to solve the problems that the existing bone-feeling style finishing agents have poor stability, cannot have both soft feel and appropriate stiffness and rigidity, do not meet the market requirements for bone-feeling style, need to be compounded with stiffeners and silicone oil on-site for use, have complex processes, are not easy to promote and apply, and have problems such as excessive formaldehyde and easy disappearance of stiffness and rigidity style.

[0006] To achieve the above-mentioned purpose, the present application provides a finishing agent for skinny style finishing, which is prepared by using 100 to 120 parts by weight of vinyl acetate monomer, 5 to 15 parts by weight of polyvinyl alcohol, 10 to 30 parts by weight of acrylate, and 5 to 25 parts by weight of multifunctional acrylic monomer as raw materials, carrying out emulsion polymerization under the joint action of a crosslinking agent, a buffer, an emulsifier and an initiator, and adding a block silicone oil in the later stage of the reaction;

[0007] Wherein, the weight ratio of the cross-linking agent to the multifunctional acrylic monomer is (0.8-1.5):1.

[0008] Preferably, the above-mentioned block silicone oil is a multi-polymer hydrophilic block silicone oil.

[0009] More preferably, the mass percentage of the block silicone oil in the finishing agent is 25wt% to 55wt%.

[0010] Preferably, the multifunctional acrylic monomer is selected from one or more of diallyl phthalate, diethylene glycol diacrylate, tripropylene glycol diacrylate, triallyl cyanurate, trimethylolpropane triacrylate, pentaerythritol triacrylate and dipentaerythritol hexaacrylate.

[0011] Preferably, the crosslinking agent is selected from one or more of hydroxyethyl acrylamide, N-(isobutyloxy)methacrylamide, hydroxypropyl methacrylate, hydroxypropyl acrylate, acrylic acid, methacrylic acid, acrylamide and diacetone acrylamide.

[0012] Preferably, the above-mentioned polyvinyl alcohol is selected from one or more of polyvinyl alcohol 0488, polyvinyl alcohol 0588, polyvinyl alcohol 0788, polyvinyl alcohol 1088, polyvinyl alcohol 1788, polyvinyl alcohol 2088 and polyvinyl alcohol 2488.

[0013] Preferably, the acrylic acid ester is selected from one or more of butyl acrylate, butyl methacrylate, ethyl acrylate, methyl acrylate, methyl methacrylate and versatate.

[0014] Preferably, the above-mentioned multi-polymer hydrophilic block silicone oil is one or more of the block silicone oils TF-463, TF-4511B, TF-4881C, TF-4563A, TF-4826 and TF-4550C produced by Transfar Intelligent Technology Co., Ltd.

[0015] Another object of the present application is to provide a method for preparing the above-mentioned finishing agent, comprising the following steps:

[0016] S1, dissolving the polyvinyl alcohol in water to prepare a protective glue solution;

[0017] S2, preparing a mixed monomer by mixing the vinyl acetate monomer, acrylate, crosslinking agent and multifunctional acrylic monomer;

[0018] S3, mixing the protective glue solution, the mixed monomer, the buffer, the emulsifier and the initiator to carry out emulsion polymerization reaction, and adding the block silicone oil in the later stage of the reaction to obtain a finishing agent.

[0019] Preferably, in step S3, the mixing step comprises: adding the mixed monomer, buffer, emulsifier and initiator to the protective colloid solution at one time or in batches.

[0020] Preferably, the above-mentioned batch addition method is as follows:

[0021] The protective gel solution, buffer, emulsifier and part of the mixed monomer are mixed, and the temperature is raised to 65°C to 75°C. A part of the initiator is added, and the temperature is further raised to 75°C to 78°C, and the temperature is kept for 20min to 40min. The remaining initiator and the remaining mixed monomer are added, and the initiator is added 10min to 15min later than the mixed monomer to obtain a reaction solution.

[0022] Preferably, the above-mentioned partial mixed monomer accounts for 10% to 15% of the total mass of the mixed monomer.

[0023] Preferably, the above-mentioned partial initiator accounts for 45% to 50% of the total mass of the above-mentioned initiator.

[0024] Preferably, the remaining initiator and the remaining mixed monomer are added dropwise for 4 to 7 hours at a reaction temperature of 75°C to 80°C.

[0025] Preferably, after the addition of the above initiator is completed, the temperature is kept for 20 to 40 minutes to obtain a reaction solution.

[0026] Preferably, the temperature of the reaction liquid is controlled at 60° C. to 70° C., the block silicone oil is added and stirred to mix, and then the temperature is lowered and filtered to obtain the finishing agent.

[0027] The present application also provides the use of the above finishing agent in the skinny style finishing of fabrics.

[0028] In general, the above technical solutions conceived by this application have the following technical advantages compared with the prior art:

[0029] (1) The finishing agent for skinny style finishing provided by the present application is prepared by using vinyl acetate monomer, polyvinyl alcohol, acrylate and multifunctional acrylic monomer as raw materials, carrying out emulsion polymerization under the joint action of crosslinking agent, buffer, emulsifier and initiator, and adding block silicone oil in the later stage of the reaction. The finishing agent does not contain formaldehyde and has good stability. The fabric finished by the finishing agent can have excellent toughness, soft hand feel and appropriate stiffness, meeting the customer's requirements for skinny style.

[0030] (2) In the preferred embodiment, the present application strengthens the cross-linking effect of vinyl acetate monomer, polyvinyl alcohol and acrylate by adjusting the formula, and controls the amount of multifunctional acrylic acid monomer, so that the reaction raw materials are polymerized to form a polymer with a spatial network structure, reshaping the skeleton structure of the finishing agent, so that the fabric after finishing can maintain stiffness. At the same time, the non-ionic emulsifier, block silicone oil and other components are coordinated to improve the stability of the finishing agent, and the two functions of softness and stiffness can be directly integrated into the finishing agent at the same time. Users do not need to temporarily add silicone oil when using it. Only using the finishing agent alone can achieve the skinny style required by customers, effectively solving the problems of excessive formaldehyde, complex use process, and many additives in the skinny style finishing of textiles. DETAILED DESCRIPTION

[0031] In order to make the purpose, technical solution and advantages of the present application more clear, the present application is further described in detail below in conjunction with the embodiments. It should be understood that the specific embodiments described here are only used to explain the present application and are not used to limit the present application.

[0032] The present application provides a finishing agent for skinny style finishing, which is prepared by using 100 to 120 parts by weight of vinyl acetate monomer, 5 to 15 parts by weight of polyvinyl alcohol, 10 to 30 parts by weight of acrylate and 5 to 25 parts by weight of multifunctional acrylic monomer as raw materials, carrying out emulsion polymerization under the joint action of a crosslinking agent, a buffer, an emulsifier and an initiator, and adding a block silicone oil in the later stage of the reaction;

[0033] Wherein, the weight ratio of the cross-linking agent to the multifunctional acrylic monomer is (0.8-1):1.

[0034] The finishing agent for skinny style finishing provided by the present application introduces a multifunctional acrylic monomer, which is combined with polyvinyl alcohol, vinyl acetate monomer, acrylate and other ingredients to form a complete skinny style finishing agent formula. The fabric finished by the finishing agent can have excellent toughness, soft hand feel and certain stiffness. Experiments have found that the stability of the finishing agent and the skinny style finishing effect are significantly better than those of stiffening agents (such as melamine resin or white latex). The two functions of soft hand feel and stiffness can be directly integrated into the finishing agent at the same time. Users do not need to temporarily add silicone oil or other additives when using it. The use process is simple and convenient, and it has a wide range of applicability.

[0035] It is understood that the multifunctional acrylic monomer is also called (meth) acrylic acid polyol ester, which is a monomer obtained by esterification of (meth) acrylic acid and polyol, and contains two or more (meth) acrylate functional groups in the molecule. In some embodiments, the multifunctional acrylic monomer is selected from one or more of diallyl phthalate, diethylene glycol diacrylate, tripropylene glycol diacrylate, triallyl cyanurate, trimethylolpropane triacrylate, pentaerythritol triacrylate and dipentaerythritol hexaacrylate.

[0036] In the present application, the crosslinking agent can undergo polymerization reaction with vinyl acetate and acrylate through carbon-carbon double bonds, and the active groups contained in the crosslinking agent itself, such as hydroxyl, carboxyl, amide, etc., can undergo polycondensation crosslinking reaction. In some embodiments, the crosslinking agent is selected from one or more of hydroxyethyl acrylamide, N-(isobutyloxy)methacrylamide, hydroxypropyl methacrylate, hydroxypropyl acrylate, acrylic acid, methacrylic acid, acrylamide and diacetone acrylamide.

[0037] In some embodiments, in the above raw materials, the weight ratio of the sum of vinyl acetate monomer and acrylate to multifunctional acrylic monomer is (5-30):1, preferably (6-26):1, which can enable the reaction raw materials to polymerize to form a polymer with a network structure, thereby reshaping the skeleton structure of the finishing agent.

[0038] In some embodiments, the block silicone oil is a multi-component (ternary or above) copolymerized hydrophilic block silicone oil. Experiments have found that when the block silicone oil is other types of block silicone oils, such as amino-modified block silicone oils, the stability of the prepared finishing agent is poor. This application does not limit the source of the multi-component copolymerized hydrophilic block silicone oil, which can be prepared in the laboratory or purchased from commercial products, such as but not limited to the block silicone oils TF-463, TF-4511B, TF-4881C, TF-4563A, TF-4826, TF-4550C, etc. produced by Chuanhua Zhilian Co., Ltd.

[0039] In order to make the finishing agent have both better toughness and softer feel, in some embodiments, the mass percentage of the block silicone oil in the finishing agent is 25wt% to 55wt%.

[0040] In some embodiments, the polyvinyl alcohol is selected from one or more of polyvinyl alcohol 0488, polyvinyl alcohol 0588, polyvinyl alcohol 0788, polyvinyl alcohol 1088, polyvinyl alcohol 1788, polyvinyl alcohol 2088 and polyvinyl alcohol 2488. It can be understood that the first two digits 04 in 0488 represent the degree of polymerization, and the last two digits 88 represent the degree of alcoholysis, and other types of polyvinyl alcohol can be deduced accordingly.

[0041] In some embodiments, the acrylic acid ester is selected from one or more of butyl acrylate, butyl methacrylate, ethyl acrylate, methyl acrylate, methyl methacrylate and versatate.

[0042] In some embodiments, the initiator is one or more of sodium persulfate, potassium persulfate and ammonium persulfate. In some embodiments, the amount of the initiator is 0.4 to 1 part.

[0043] In some embodiments, the buffer is sodium bicarbonate or sodium acetate. In some embodiments, the amount of the buffer is 0.1 to 0.3 parts.

[0044] In some embodiments, the emulsifier is a cationic emulsifier or a nonionic emulsifier. In some embodiments, the emulsifier is used in an amount of 0.5 to 3 parts.

[0045] In some embodiments, the nonionic emulsifier includes but is not limited to fatty alcohol polyoxyethylene ether.

[0046] In some embodiments, the fatty alcohol polyoxyethylene ether is selected from one or more of the AEO series and the isomeric tridecanol polyoxyethylene ether series. The fatty alcohol polyoxyethylene ether (AEO), also known as polyoxyethylene fatty alcohol ether, is an ether formed by condensation of polyethylene glycol (PEG) and fatty alcohol, and is represented by the following general formula: RO(CH2CH2O) n H, wherein R is a saturated or unsaturated C12-C18 hydrocarbon group, which can be a straight-chain hydrocarbon group or a branched hydrocarbon group; n is the addition number of ethylene oxide, that is, the number of ethylene oxide groups in the molecule. Due to the different degrees of polymerization of polyethylene glycol and the types of fatty alcohols, there are different varieties. The value range of n in the molecule of the present application is 3-15. It can be understood that AEO9 means that n is 9, and other types of fatty alcohol polyoxyethylene ethers can be deduced accordingly.

[0047] On the other hand, the present application also provides a method for preparing the above finishing agent, comprising the following steps:

[0048] S1, dissolving the polyvinyl alcohol in water to prepare a protective glue solution;

[0049] S2, preparing a mixed monomer by mixing the vinyl acetate monomer, acrylate, crosslinking agent and multifunctional acrylic monomer;

[0050] S3, mixing the protective glue solution, the mixed monomer, the buffer, the emulsifier and the initiator to carry out emulsion polymerization reaction, and adding the block silicone oil in the later stage of the reaction to obtain a finishing agent.

[0051] In some embodiments, step S1 is specifically as follows: dissolving polyvinyl alcohol in deionized water, heating to 90° C. to 95° C., and keeping the temperature for 1 h to 2 h, so that the polyvinyl alcohol can be better dissolved in water, and then cooling and filtering to obtain a protective glue solution.

[0052] In some embodiments, the mass percentage of polyvinyl alcohol in the protective glue solution is 5% to 15%.

[0053] In some embodiments, in the above-mentioned mixed monomer, the mass percentage of vinyl acetate monomer is 60% to 86%, the mass percentage of acrylate is 7% to 20%, the mass percentage of cross-linking agent is 3% to 12%, and the mass percentage of multifunctional acrylic monomer is 3% to 15%.

[0054] In some embodiments, in order to make the emulsion polymerization reaction more gentle and fully reacted, the above-mentioned initiator can be first dissolved in deionized water to prepare an initiator drop solution, and then mixed with the above-mentioned protective colloid solution, mixed monomer, buffer, and emulsifier. In some embodiments, the mass percentage of the initiator in the above-mentioned initiator drop solution is 2% to 5%.

[0055] In some embodiments, in step S3, the mixing step includes: adding the mixed monomer, buffer, emulsifier and initiator to the protective glue solution at one time or in batches. In order to better control the stability of the finishing agent, it is preferred that the mixed monomer, buffer, emulsifier and initiator are added to the protective glue solution in batches.

[0056] In some embodiments, the above-mentioned batch addition method is as follows:

[0057] The protective gel solution, the buffer, the emulsifier and part of the mixed monomer are mixed, and the temperature is raised to 65°C to 75°C. A part of the initiator is then added, and the temperature is continued to be raised to 75°C to 78°C, and the temperature is kept for 20min to 40min. The remaining initiator and the remaining mixed monomer are added, and the initiator is added 10min to 15min later than the mixed monomer to obtain a reaction solution.

[0058] In some embodiments, the partial mixed monomers account for 10% to 15% of the total mass of the mixed monomers.

[0059] In some embodiments, the above-mentioned partial initiator is 45% to 50% of the total mass of the above-mentioned initiator.

[0060] In some embodiments, the remaining initiator and the remaining mixed monomer are added dropwise for 4 to 7 hours at a reaction temperature of 75°C to 80°C.

[0061] In some embodiments, in order to allow the emulsion polymerization reaction to proceed fully, after the addition of the above-mentioned initiator is completed, the temperature is kept for 20 minutes to 40 minutes to obtain a reaction solution.

[0062] In some embodiments, the temperature of the reaction solution is controlled at 60° C. to 70° C., the block silicone oil is added and stirred to mix, and then the temperature is lowered and filtered to obtain a finishing agent.

[0063] In some embodiments, after adding the above-mentioned block silicone oil and stirring and mixing, the obtained product is cooled to below 40° C. and filtered to obtain the finishing agent.

[0064] On the other hand, the present application also provides the use of the above finishing agent in the skinny style finishing of fabrics.

[0065] In some embodiments, when the above finishing agent is used to finish the fabric, the following steps are included: immersing the fabric in the above finishing agent, performing padding and shaping.

[0066] In some embodiments, the above-mentioned dipping and rolling method is selected from one dipping and one rolling, two dipping and two rolling, or multiple dipping and multiple rolling. Those skilled in the art can adjust it according to the liquid carrying rate of the fabric during the dipping and rolling process, which is within the protection scope of this application.

[0067] Based on this, the present application also provides a fabric with a skinny style, which is obtained after being finished by the above-mentioned fabric finishing method.

[0068] The finishing agent provided in the present application is used to perform skinny style finishing on fabrics, and the toughness, softness and drape of the fabrics are significantly improved. The fabrics have excellent toughness and soft hand feel, while having appropriate stiffness, meeting the market requirements for skinny style.

[0069] It should be understood that materials of the same or similar type, model, quality, nature or function as the reagents and instruments used in the following examples can be used to implement the present application. The experimental methods used in the following examples are conventional methods unless otherwise specified. The materials, reagents, etc. used in the following examples can be obtained from commercial sources unless otherwise specified.

[0070] The following are examples and comparative examples:

[0071] Example 1

[0072] The finishing agent provided in this embodiment is prepared from the following components:

[0073] 5 parts of polyvinyl alcohol (brand 1788), 120 parts of deionized water, 120 parts of vinyl acetate, 10 parts of acrylate (ethyl acrylate), 5 parts of multifunctional acrylic monomer (diethylene glycol diacrylate), 5 parts of crosslinking agent (N-(isobutyloxy) methacrylamide), 0.4 parts of initiator (potassium persulfate), 0.1 parts of buffer (sodium bicarbonate), 0.5 parts of non-ionic emulsifier (AEO-9) and 40 parts of block silicone oil (TF-463 produced by Chuanhua Zhilian Co., Ltd.).

[0074] The preparation method of the finishing agent provided in this embodiment comprises the following steps:

[0075] S1. Dissolve polyvinyl alcohol in 100 parts of deionized water, raise the temperature to 90°C, keep the temperature for 1 hour, then cool to room temperature, filter to remove insoluble impurities, and obtain a protective glue solution;

[0076] S2, stirring and mixing vinyl acetate, acrylic acid ester, multifunctional acrylic monomer and crosslinking agent to obtain a mixed monomer;

[0077] S3, dissolving the initiator in 20 parts of deionized water to obtain an initiator drop solution;

[0078] S4. Add the above-mentioned protective gel solution, buffer, non-ionic emulsifier and 20 parts of mixed monomers into a glass flask, heat to 65°C, then add 10 parts of initiator droplets at a time, continue to heat to 75°C and keep warm for 30 minutes; then add the remaining initiator droplets and the remaining mixed monomers dropwise, the addition time is 4 hours, the reaction temperature is 75°C, and the initiator droplets are added 10 minutes later than the mixed monomers; after all the additions are completed, keep warm for 30 minutes to obtain a reaction solution.

[0079] S5. When the reaction liquid is cooled to 60°C, block silicone oil is added and stirred evenly. When the reaction liquid is cooled to 40°C, it is filtered to obtain a finishing agent.

[0080] Example 2

[0081] The finishing agent provided in this embodiment is prepared from the following components:

[0082] 15 parts of polyvinyl alcohol (5 parts of polyvinyl alcohol 1788, 10 parts of polyvinyl alcohol 0788), 120 parts of deionized water, 100 parts of vinyl acetate, 30 parts of acrylate (methyl methacrylate), 10 parts of multifunctional acrylic monomer (trimethylolpropane triacrylate), 15 parts of crosslinking agent (hydroxyethyl acrylamide), 0.5 parts of initiator (potassium persulfate), 0.3 parts of buffer (sodium bicarbonate), 3 parts of non-ionic emulsifier (AEO-6) and 60 parts of block silicone oil (TF-4511B produced by Chuanhua Zhilian Co., Ltd.).

[0083] The preparation method of the finishing agent provided in this embodiment comprises the following steps:

[0084] S1. Dissolve polyvinyl alcohol in 100 parts of deionized water, raise the temperature to 95°C, keep the temperature for 1 hour, then cool to room temperature, filter to remove insoluble impurities, and obtain a protective glue solution;

[0085] S2, stirring and mixing vinyl acetate, acrylic acid ester, multifunctional acrylic monomer and non-aldehyde crosslinking agent to obtain a mixed monomer;

[0086] S3, dissolving the initiator in 20 parts of deionized water to obtain an initiator drop solution;

[0087] S4. Add the above-mentioned protective gel solution, buffer, non-ionic emulsifier and 20 parts of mixed monomers into a glass flask, heat to 70°C, then add 10 parts of initiator droplets at a time, continue to heat to 75°C and keep warm for 30 minutes; then add the remaining initiator droplets and the remaining mixed monomers dropwise, the addition time is 4 hours, the reaction temperature is 78°C, and the initiator droplets are added 15 minutes later than the mixed monomers; after all the additions are completed, keep warm for 30 minutes to obtain a reaction solution.

[0088] S5. When the reaction liquid is cooled to 70°C, block silicone oil is added and stirred evenly. When the reaction liquid is cooled to 40°C, it is filtered to obtain a finishing agent.

[0089] Example 3

[0090] The finishing agent provided in this embodiment is prepared from the following components:

[0091] 15 parts of polyvinyl alcohol (polyvinyl alcohol 2488), 140 parts of deionized water, 120 parts of vinyl acetate, 30 parts of acrylate (vinyl ester), 25 parts of multifunctional acrylic monomer (trimethylolpropane triacrylate), 20 parts of crosslinking agent (diacetone acrylamide), 1 part of initiator (potassium persulfate), 0.3 parts of buffer (sodium bicarbonate), 3 parts of non-ionic emulsifier (AEO-3) and 100 parts of block silicone oil (TF-4563A produced by Chuanhua Zhilian Co., Ltd.).

[0092] The preparation method of the finishing agent provided in this embodiment comprises the following steps:

[0093] S1. Dissolve polyvinyl alcohol in 100 parts of deionized water, raise the temperature to 95°C, keep the temperature for 1 hour, then cool to room temperature, filter to remove insoluble impurities, and obtain a protective glue solution;

[0094] S2, stirring and mixing vinyl acetate, acrylic acid ester, multifunctional acrylic monomer and non-aldehyde crosslinking agent to obtain a mixed monomer;

[0095] S3, dissolving the initiator in 20 parts of deionized water to obtain an initiator drop solution;

[0096] S4. Add the above-mentioned protective glue solution, buffer, non-ionic emulsifier and 20 parts of mixed monomers into a glass flask, heat to 73°C, then add 10 parts of initiator droplets at a time, continue to heat to 78°C and keep warm for 30 minutes; then add the remaining initiator droplets and the remaining mixed monomers dropwise, the addition time is 4.5 hours, the reaction temperature is 80°C, and the initiator droplets are added 15 minutes later than the mixed monomers; after all the additions are completed, keep warm for 30 minutes to obtain a reaction solution.

[0097] S5. When the reaction liquid is cooled to 70°C, block silicone oil is added and stirred evenly. When the reaction liquid is cooled to 40°C, it is filtered to obtain a finishing agent.

[0098] Comparative Example 1

[0099] The preparation method of the finishing agent provided in this comparative example comprises the following steps: 160 g of melamine resin (TF-6320) and 100 g of block silicone oil (TF-4563A produced by Chuanhua Zhilian Co., Ltd.) are uniformly mixed and applied on site to obtain a finishing agent.

[0100] Comparative Example 2

[0101] The preparation method of the finishing agent provided in this comparative example comprises the following steps: 350 g of white glue (TF-6350) and 100 g of block silicone oil (TF-4563A produced by Chuanhua Zhilian Co., Ltd.) are uniformly mixed and applied on site to obtain a finishing agent.

[0102] Comparative Example 3

[0103] The formula of the finishing agent provided in this comparative example does not contain a multifunctional acrylic monomer, and the other components are the same as those in Example 1.

[0104] Comparative Example 4

[0105] The formula of the finishing agent provided in this comparative example does not contain block silicone oil, and the other aspects are the same as those of Example 1.

[0106] Comparative Example 5

[0107] The formula of the finishing agent provided in this comparative example does not contain multifunctional acrylic monomers and block silicone oil, and the rest is the same as in Example 1.

[0108] Comparative Example 6

[0109] No crosslinking agent is added to the formula of the finishing agent provided in this comparative example, and the rest is the same as in Example 1.

[0110] Comparative Example 7

[0111] The finishing agent provided in this comparative example is prepared from the following components:

[0112] 5 parts of polyvinyl alcohol (brand 1788), 120 parts of deionized water, 120 parts of vinyl acetate, 10 parts of acrylate (ethyl acrylate), 5 parts of multifunctional acrylic monomer (diethylene glycol diacrylate), 10 parts of crosslinking agent (N-(isobutyloxy) methacrylamide), 0.4 parts of initiator (potassium persulfate), 0.1 parts of buffer (sodium bicarbonate), 0.5 parts of non-ionic emulsifier (AEO-9) and 40 parts of block silicone oil (TF-463 produced by Chuanhua Zhilian Co., Ltd.).

[0113] During the preparation process, it was found that when the amount of the cross-linking agent used was too much, the above raw materials produced gel during the polymerization reaction and could not be compounded with the block silicone oil to obtain the finishing agent.

[0114] The fabrics were subjected to bone finishing using the finishing agents provided in Examples 1 to 3 and Comparative Examples 1 to 6, respectively, and the toughness, softness, drape and free formaldehyde content of the fabrics after bone finishing were tested. The process flow of the fabric bone finishing is shown below, and the test results are shown in Table 1:

[0115] Fabric preparation (original fabric: polyester brushed fabric) → liquid preparation (dissolve the finishing agent in deionized water to obtain a padding solution, the concentration of the finishing agent is 60g / L) → padding → shaping (180℃×60s) → fabric drop → moisture regain → evaluation.

[0116] Toughness, drape, and softness: Tested in accordance with the standard AATCC 202-2014 "Relative Hand Values ​​of Textiles: Instrumental Method", in which the larger the value of each measurement, the stronger the characteristics of the sample. For example, the larger the toughness value, the stronger the toughness and elasticity of the fabric; the larger the softness value, the softer the fabric; the larger the drape value, the harder the fabric.

[0117] Free formaldehyde content in fabric: Tested in accordance with standard GB / T 2912.1-2009 “Determination of formaldehyde in textiles - Part 1: Free and hydrolyzed formaldehyde (water extraction method)”.

[0118] Table 1 Performance test results of fabrics treated with finishing agents

[0119]

[0120]

[0121] It can be seen from Table 1 that, compared with the original fabric, the toughness, softness and drape of the fabric after being finished in a skinny style with the finishing agent provided by the present application are significantly improved, indicating that the fabric has excellent toughness and soft hand feel, and at the same time has appropriate stiffness, meeting the market requirements for a skinny style.

[0122] The toughness, softness and drape of the fabric finished with the finishing agent (Comparative Example 1) prepared on-site by melamine and silicone oil can reach the level of the embodiment of the present application, but the free formaldehyde content on the fabric surface reaches 56 mg / kg, which exceeds the formaldehyde standard and does not meet the environmental protection requirements. In addition, the finishing agent needs to be prepared on-site, and the use process is complicated, which is not convenient for promotion and application. The toughness and drape of the fabric finished with the finishing agent (Comparative Example 2) prepared on-site by white glue and silicone oil are significantly lower than those of the embodiment of the present application, and the soft feel and stiffness cannot be balanced, and the fabric cannot be given a skinny style. In addition, the finishing agent also needs to be prepared and used immediately, and the use process is complicated, which is not convenient for promotion and application.

[0123] The finishing agent for skinny style finishing provided by the present application uses vinyl acetate monomer, polyvinyl alcohol, acrylate, cross-linking agent and multifunctional acrylic monomer as raw materials, carries out emulsion polymerization reaction under the joint action of buffer, emulsifier and initiator, and is prepared by adding block silicone oil in the later stage of the reaction. It can react to form a polymer with a spatial network result, so that the stiffness of the finishing agent can be maintained after the fabric is finished and formed into a film. The finishing agent has high stability and can directly integrate both softness and stiffness functions into the finishing agent. Users do not need to temporarily add silicone oil when using it. Only the finishing agent alone can achieve the skinny style required by the customer, effectively solving the problems of excessive formaldehyde, complicated use process, and many additives in the skinny style finishing of textiles.

[0124] It will be easily understood by those skilled in the art that the above description is only a preferred embodiment of the present application and is not intended to limit the present application. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present application shall be included in the scope of protection of the present application.

Claims

1. A finishing agent for skinny style finishing, characterized in that: The finishing agent is prepared by using 100 to 120 parts by weight of vinyl acetate monomer, 5 to 15 parts by weight of polyvinyl alcohol, 10 to 30 parts by weight of acrylate, and 5 to 25 parts by weight of multifunctional acrylic monomer as raw materials, and carrying out emulsion polymerization reaction under the joint action of a crosslinking agent, a buffer, an emulsifier and an initiator, and adding a block silicone oil in the later stage of the reaction; Wherein, the weight ratio of the cross-linking agent to the multifunctional acrylic monomer is (0.8-1.5):

1.

2. The finishing agent according to claim 1, characterized in that The block silicone oil is a multi-polymer hydrophilic block silicone oil; Preferably, the mass percentage of the block silicone oil in the finishing agent is 25wt% to 55wt%.

3. The finishing agent according to claim 1, characterized in that The multifunctional acrylic monomer is selected from one or more of diallyl phthalate, diethylene glycol diacrylate, tripropylene glycol diacrylate, triallyl cyanurate, trimethylolpropane triacrylate, pentaerythritol triacrylate and dipentaerythritol hexaacrylate; and / or, The crosslinking agent is selected from one or more of hydroxyethyl acrylamide, N-(isobutyloxy)methacrylamide, hydroxypropyl methacrylate, hydroxypropyl acrylate, acrylic acid, methacrylic acid, acrylamide and diacetone acrylamide.

4. The finishing agent according to claim 1, characterized in that The polyvinyl alcohol is selected from one or more of polyvinyl alcohol 0488, polyvinyl alcohol 0588, polyvinyl alcohol 0788, polyvinyl alcohol 1088, polyvinyl alcohol 1788, polyvinyl alcohol 2088 and polyvinyl alcohol 2488; and / or, The acrylic acid ester is selected from one or more of butyl acrylate, butyl methacrylate, ethyl acrylate, methyl acrylate, methyl methacrylate and versatate; and / or, The multi-polymer hydrophilic block silicone oil is one or more of the block silicone oils TF-463, TF-4511B, TF-4881C, TF-4563A, TF-4826 and TF-4550C produced by Transfar Intelligent Technology Co., Ltd.

5. The method for preparing the finishing agent according to any one of claims 1 to 4, characterized in that: The steps include: S1, dissolving the polyvinyl alcohol in water to prepare a protective glue solution; S2, preparing a mixed monomer from the vinyl acetate monomer, acrylate, a crosslinking agent and a multifunctional acrylic monomer; S3, mixing the protective glue solution, the mixed monomer, the buffer, the emulsifier and the initiator to carry out emulsion polymerization reaction, and adding the block silicone oil in the later stage of the reaction to obtain a finishing agent.

6. The preparation method according to claim 5, characterized in that: In step S3, the mixing step includes: adding the mixed monomer, buffer, emulsifier and initiator to the protective colloid solution at one time or in batches.

7. The preparation method according to claim 6, characterized in that: The method of adding in batches is as follows: The protective gel solution, the buffer, the emulsifier and part of the mixed monomer are mixed, and the temperature is raised to 65°C to 75°C. A part of the initiator is then added, and the temperature is continued to be raised to 75°C to 78°C, and the temperature is kept for 20min to 40min. The remaining initiator and the remaining mixed monomer are added, and the initiator is added 10min to 15min later than the mixed monomer to obtain a reaction solution.

8. The preparation method according to claim 7, characterized in that: The partial mixed monomers are 10% to 15% of the total mass of the mixed monomers; The partial initiator is 45% to 50% of the total mass of the initiator; The remaining initiator and the remaining mixed monomer are added dropwise for 4 to 7 hours at a reaction temperature of 75 to 80°C; After the initiator is added, the mixture is kept warm for 20 to 40 minutes to obtain a reaction solution.

9. The preparation method according to claim 8, characterized in that: The temperature of the reaction liquid is controlled at 60° C. to 70° C., the block silicone oil is added and stirred to mix, and then the temperature is lowered and filtered to obtain a finishing agent.

10. Use of the finishing agent according to any one of claims 1 to 4 in the skinny style finishing of fabrics.

Citation Information

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