Silk finishing liquid and treatment method using the same

Abstract

The present application relates to the technical field of silk finishing, and in particular to a silk finishing liquid and a treatment method using the silk finishing liquid; wherein, a silk finishing liquid comprises a microcapsule mixture, an adhesive, a cross-linking agent and an organic acid; the microcapsule mixture is a mixture of microcapsules with skin care oil as a core material and polyurethane as a wall material; the microcapsules containing the skin care oil are bonded to the silk fabric through an adhesive, and mesoporous material is added to the wall material of the microcapsule to enhance the strength of the polyurethane wall material and reduce the rupture of the microcapsules during the washing and wearing processes of the silk fabric; at the same time, the skin care oil in the microcapsule is slowly released through the mesoporous material, thereby enhancing the moisturizing effect of the silk fabric and the washability of the skin care oil in the silk fabric.

Description

Technical Field

[0001] The present application relates to the technical field of silk finishing, and in particular to a silk finishing liquid and a treatment method using the silk finishing liquid. Background Art

[0002] Skin care oil is a commonly used skin care health product. If it is applied to silk fabrics through certain methods to prepare textiles with moisturizing and skin care functions, it conforms to the healthy living concept of modern consumers and meets people's demand for health-care functional textiles.

[0003] In the existing finishing process of adding skin care oil to silk fabrics, the wash resistance of the skin care oil in the prepared silk fabrics is not ideal. The initial skin care oil content of the finished silk fabrics is often high, and a large amount of skin care oil is lost during washing, which cannot achieve long-term skin care effects. Summary of the Invention

[0004] In order to overcome the problem that the skin care oil in the silk fabric prepared by the existing finishing process of adding the skin care oil to the silk fabric has unsatisfactory wash resistance, the present application provides a silk finishing liquid and a treatment method using the silk finishing liquid.

[0005] In a first aspect, the present application provides a silk finishing liquid, which adopts the following technical solution:

[0006] A silk finishing liquid comprises, by weight, 15-30 parts of a microcapsule mixture, 10-30 parts of an adhesive, 2-5 parts of a cross-linking agent, 30-40 parts of water, and 0.4-0.8 parts of a catalyst;

[0007] The microcapsule mixture is a mixture of microcapsules with skin care oil as the core material and polyurethane as the wall material; the raw materials of the microcapsule mixture include 100-150 parts of polyether diol, 100-110 parts by mass of diisocyanate, 4-8 parts of glycerol, 0.1-0.2 parts of catalyst, 8-15 parts of dimethylol propionic acid, 8-15 parts of acetone, 2-5 parts of triethylamine, 3-8 parts of ethylenediamine, 120-150 parts of skin care oil, 10-20 parts of mesoporous material and 800 parts of water;

[0008] The mesoporous material is one of mesoporous silica, nano zeolite and nano bentonite.

[0009] By adopting the above technical solution, the microcapsules use polyurethane as the wall material, and mesoporous material is added to the polyurethane wall material, and the microcapsules of the skin care oil are arranged on the silk fabric through a binder.

[0010] By adding mesoporous materials to the wall materials of polyurethane: on the one hand, the strength of the polyurethane wall materials is enhanced, reducing the rupture of microcapsules in silk fabrics during the washing and wearing process; on the other hand, the skin care oil in the microcapsules is slowly released through the mesoporous materials, thereby improving the skin care effect of the finished silk fabrics and the washability of the skin care oil in the silk fabrics.

[0011] Preferably, the raw materials of the microcapsule mixture further include 30-60 parts by mass of hydroxyl-terminated polydimethylsiloxane; the preparation process of the microcapsule mixture is as follows:

[0012] Preparation of polyurethane prepolymer: polyether diol, hydroxyl-terminated polydimethylsiloxane, mesoporous material and glycerol are mixed to form a mixed solution, the mixed solution is heated to 70-90°C, diphenylmethane diisocyanate is added under nitrogen protection and stirring at 300-500 rpm, and the reaction is carried out for 0.6-1.2 hours to prepare a polyurethane prepolymer;

[0013] Salt formation and emulsification: After adding dimethylolpropionic acid to the polyurethane prepolymer, react under stirring for 1.5-2.5 hours; then cool and add acetone; then add skin care oil and triethylamine, react under stirring at 3000-5000 r / min for 1 hour, cool and add water at 5000-8000 r / min for emulsification; then add ethylenediamine for chain extension, raise the temperature to 70-90°C, and react under stirring at 500-700 r / min for 0.5-1 hour to prepare a micro-capsule mixture.

[0014] By adopting the above technical solution, hydroxyl-terminated polydimethylsiloxane is added to the wall material of the microcapsule, the siloxy bonds can rotate freely, and there is a concentration difference of the moisturizing oil inside and outside the microcapsule; under the combined effect of the concentration difference, the easy free rotation of the siloxy bonds and the sustained-release effect of the mesoporous material, more moisturizing oil can be sustained-released through the wall material of the microcapsule, so that the prepared silk fabric has excellent moisturizing effect and water-resistant performance of the moisturizing effect, and the moisturizing oil is not easy to form oil spots on the silk fabric.

[0015] Preferably, the skin care oil is at least one of olive oil, aloe vera oil, vitamin E and vitamin C.

[0016] By adopting the above technical solution, by adding moisturizing oil into the microcapsules, the microcapsules can slowly release the moisturizing oil, thereby making the silk fabric have a moisturizing effect.

[0017] Preferably, the silk finishing liquid contains at least one microcapsule.

[0018] By adopting the above technical solution, microcapsules containing different types of moisturizing oils are prepared, and different microcapsules are used in combination to further improve the moisturizing effect of the prepared silk fabric.

[0019] Preferably, the adhesive is water-based polyurethane.

[0020] Water-based polyurethane is preferred, as it not only has good bonding properties and yellowing resistance on silk fabrics but also has a good hand feel.

[0021] Preferably, the crosslinking agent is one of a silane crosslinking agent, triethylamine and butanetetracarboxylic acid.

[0022] By adopting the above technical solution, the addition of a cross-linking agent further enhances the strength of the film layer formed by the adhesive on the silk fabric, and enhances the bonding force between the microcapsules and the film layer formed by the adhesive, thereby improving the moisturizing effect of the prepared silk fabric and the wash resistance of the moisturizing effect.

[0023] Preferably, the silane crosslinking agent is one of dodecyltriethoxysilane, methyltrimethoxysilane, propyltriacetoxysilane and propyltriacetoxysilane.

[0024] By adopting the above technical solution, a silane crosslinking agent is used in the silk finishing liquid to improve the softness of the silk fabric and reduce the damage of the silk fabric during use or washing. Alkyl triethoxy, methyl trimethoxy, propyl triacetoxy silane, and propyl triacetoxy silane are preferred. The silk fabric is not easy to turn yellow during use and the gloss of the silk fabric is better maintained.

[0025] The use of silane cross-linking agent in the silk finishing liquid makes the film layer formed by the silk finishing liquid softer and fluffier, which is conducive to the uniform distribution of the moisturizing oil on the silk fabric and the sustained release of the moisturizing oil by the microcapsules, thereby improving the moisturizing effect of the prepared silk fabric and the water-washing resistance of the moisturizing effect.

[0026] Preferably, the silk finishing liquid further comprises 2-4 parts by mass of an ultraviolet absorber.

[0027] By adopting the above technical solution, an ultraviolet absorber is used in the silk finishing liquid, thereby reducing the oxidation of the silk fabric and the film layer on the silk fabric by ultraviolet rays, so that the silk fabric can better maintain the silk luster.

[0028] Preferably, the silk finishing liquid further comprises 3-8 parts by mass of titanium dioxide hydrosol;

[0029] The titanium dioxide hydrosol is a mixed solution prepared by reacting 1-3 parts by mass of n-butyl titanate and 10-15 parts by mass of water under the catalysis of acetic acid.

[0030] By adopting the above technical solution, titanium dioxide hydrosol is added to the silk finishing liquid, thereby enhancing the antioxidant and anti-ultraviolet properties of the silk fabric. Moreover, the titanium dioxide hydrosol has a high surface energy, which enhances the bonding force between the silk finishing liquid and the silk fibers, while improving the dispersion performance of the ultraviolet absorber. Furthermore, the light resistance, moisture retention and water washing resistance of the prepared silk fabric are improved, and the prepared silk fabric has a better gloss.

[0031] In a second aspect, the present application provides a method for treating silk finishing liquid.

[0032] A method for treating a silk finishing liquid comprises the following steps:

[0033] The microcapsule mixture, adhesive, cross-linking agent, water and organic acid are mixed to prepare a silk finishing solution;

[0034] The silk fabric is dried, rolled, and then impregnated with silk finishing liquid;

[0035] The padded silk fabric is tentered and then hot-air finished at 110-130° C. for 1-2 minutes to prepare a silk fabric; the silk fabric is immersed in the silk finishing liquid for 30-40 minutes; and the temperature of the silk finishing liquid during the immersion is 20-30° C.

[0036] By adopting the above technical solution, the silk fabric is treated with silk finishing liquid and then hot-air finished, and the silk finishing liquid undergoes physical and chemical changes to form a soft and high-strength film layer on the silk fabric, and the microcapsules are dispersed in the film layer; the microcapsules have high strength and the wall material of the microcapsules has mesoporous materials and polyurethane soft segments that are conducive to the sustained release of moisturizing oil. The microcapsules sustain the release of the moisturizing oil, so that the prepared silk fabric has excellent moisturizing effect and water-resistant properties with moisturizing effect.

[0037] In summary, this application has the following beneficial effects:

[0038] 1. The wall material of the microcapsule is made of polyurethane, and mesoporous material is added to the polyurethane to enhance the strength of the polyurethane wall material and reduce the rupture of microcapsules during the washing and wearing process of silk fabrics; at the same time, the skin care oil in the microcapsule is slowly released through the mesoporous material, thereby improving the moisturizing effect of the finished silk fabric and the washability of the skin care oil in the silk fabric.

[0039] 2. By adopting a silane cross-linking agent, and preferably selecting the type of silane cross-linking agent, the strength of the film formed by the silk finishing liquid, the softness and fluffiness of the silk fabric are improved, which is conducive to the contact of the slowly released moisturizing oil with the silk fabric, thereby improving the moisturizing effect of the silk fabric, the washability of the moisturizing effect and the yellowing resistance.

[0040] 3. By adding ultraviolet absorber UV531 and titanium dioxide hydrosol to the silk finishing liquid, the high specific surface energy of titanium dioxide hydrosol enhances the bonding force between the silk finishing liquid and the silk fibers, while improving the dispersion performance of the ultraviolet absorber UV531, further improving the moisturizing effect of the silk fabric, the washability of the moisturizing effect and the yellowing resistance. DETAILED DESCRIPTION

[0041] raw material

[0042] Bentonite (average particle size 13 μm), hydroxyl-terminated dimethyl silicone oil (viscosity (25°C) 20-40 mm² / s, hydroxyl content: 6-12%), mesoporous silica (average particle size 80 nm), nano-bentonite (model: DK1, supplier: Zhejiang Fenghong New Materials Co., Ltd.), water-based polyurethane (model: FS-1940A, supplier: Anhui Feimiao Chemical Industry Co., Ltd.), and water-based epoxy adhesive (brand: JT-306, supplier: Foshan Juntu New Materials Co., Ltd.).

[0043] Preparation examples of intermediates

[0044] Preparation Example 1: A microcapsule mixture, using raw materials as shown in Table 1, and its preparation process is as follows:

[0045] Preparation of polyurethane prepolymer: Polyether diol (using polyethylene glycol 1500), hydroxyl-terminated polydimethylsiloxane, mesoporous material (using mesoporous silica) and propylene glycol are added to a reactor and mixed to form a mixed liquid; then the mixed liquid is heated to 70°C, and diisocyanate (using diphenylmethane diisocyanate) and a catalyst (using dibutyltin dilaurate) are added under nitrogen protection and stirring at 500 r / min for 0.6 h to prepare a polyurethane prepolymer.

[0046] Salt formation and emulsification: dimethylolpropionic acid is added to the polyurethane prepolymer and reacted for 1.5 hours under stirring at 1000 r / min; then the temperature is lowered to 40°C and acetone is added, followed by skin care oil (a composition of aloe vera oil and vitamin E in a mass ratio of 1:1) and triethylamine, and the mixture is reacted for 1 hour under stirring at 5000 r / min. The temperature is lowered and water is added to emulsify the mixture at 5000 r / min; then ethylenediamine is added for chain extension, the temperature is raised to 70°C, and the mixture is reacted for 1 hour under stirring at 500 r / min to prepare a micro-capsule mixture.

[0047] Preparation Example 2, a microcapsule mixture, differs from Preparation Example 1 in that the weights of the raw materials used are different, as shown in Table 1; and the types of raw materials and preparation processes are different, as shown below:

[0048] Preparation of polyurethane prepolymer: Polyether diol (using polypropylene glycol 1500), hydroxyl-terminated polydimethylsiloxane, mesoporous material (using nano zeolite) and propylene glycol are added to a reactor to form a mixed liquid; then the mixed liquid is heated to 80°C, and diisocyanate (using dimethyl diphenyl diisocyanate) and a catalyst (using dibutyltin dilaurate) are added under nitrogen protection and stirring at 400 r / min for 1.0 h to prepare a polyurethane prepolymer.

[0049] Salt formation and emulsification: dimethylolpropionic acid is added to the polyurethane prepolymer and reacted for 2.0 hours under stirring at 900 r / min; then the temperature is lowered to 40°C and acetone is added, followed by skin care oil (a composition of olive oil and vitamin E in a mass ratio of 1:1) and triethylamine, and the mixture is reacted for 1 hour under stirring at 4000 r / min; then water is added for emulsification at 6000 r / min, followed by addition of ethylenediamine for chain extension, the temperature is raised to 80°C, and the mixture is reacted for 0.8 hours under stirring at 600 r / min to prepare a micro-capsule mixture.

[0050] Preparation Example 3, a microcapsule mixture, differs from Preparation Example 1 in that the weights of the raw materials used are different, as shown in Table 1; and the types of raw materials and the preparation process are different, as shown below:

[0051] Preparation of polyurethane prepolymer: Polyether diol (polyethylene glycol 1500), hydroxyl-terminated polydimethylsiloxane, mesoporous material (nanobentonite), and glycerol were added to a reaction kettle to form a mixed solution. The mixed solution was then heated to 90°C, and diisocyanate (isophorone diisocyanate) and catalyst (triethylenediamine) were added under nitrogen protection and stirring at 300 rpm. The mixture was reacted for 0.6 h to prepare a polyurethane prepolymer.

[0052] Salt formation and emulsification: dimethylolpropionic acid is added to the polyurethane prepolymer and reacted for 2.5 hours under stirring at 800 r / min; then the temperature is lowered to 30°C and acetone is added, followed by skin care oil (using vitamin E) and triethylamine, and the reaction is carried out under stirring at 3000 r / min for 1 hour; then water is added and emulsified at 8000 r / min; then ethylenediamine is added for chain extension, the temperature is raised to 70°C and the reaction is carried out at stirring at 700 r / min for 0.5 hours to prepare a micro-capsule mixture.

[0053] Table 1: List of types and weights of raw materials used in the microcapsule mixtures of Preparation Examples 1-3

[0054] distinguish Preparation Example 1 Preparation Example 2 Preparation Example 3 Polyether diol / kg 150 130 100 Hydroxyl terminated polydimethylsiloxane / kg 30 50 60 Glycerol / kg 4 6 8 Diisocyanate / kg 100 105 110 Catalyst / kg 0.1 0.15 0.2 Dimethylolpropionic acid / kg 6 10 15 Acetone / kg 15 10 8 Triethylamine / kg 2 4 5 Ethylenediamine / kg 3 6 8 Water / kg 800 800 800 Skin care oil / kg 120 130 150 Mesoporous material / kg 10 15 20

[0055] Preparation Example 4, a microcapsule mixture, differs from Preparation Example 1 in that an equal amount of polyethylene glycol 1500 is used to replace the hydroxyl-terminated polydimethylsiloxane.

[0056] Preparation Example 5, a microcapsule mixture, differs from Preparation Example 1 in that an equal amount of vitamin E is used to replace aloe vera oil in the moisturizing oil.

[0057] Preparation Example 6, a microcapsule mixture, differs from Preparation Example 1 in that an equal amount of aloe vera oil is used to replace vitamin E in the moisturizing oil.

[0058] Preparation Example 7, a titanium dioxide hydrosol, using the raw materials shown in Table 2, the preparation process is as follows:

[0059] Water and acetic acid are mixed to form a mixed solution. Tetra-n-butyl titanate is slowly added dropwise to the mixed solution under stirring at 4000 r / min. After the addition is completed within 15 minutes, the mixture is stirred for 20 minutes to form a titanium dioxide hydrosol.

[0060] Preparation Example 8-9, a titanium dioxide hydrosol, differs from Preparation Example 7 in that the weight of raw materials and parameter settings of the preparation process are different, as shown in Table 2.

[0061] Table 2 List of raw material weights and preparation process parameters for the titanium dioxide hydrosols of Preparation Examples 7-9

[0062] distinguish Preparation Example 7 Preparation Example 8 Preparation Example 9 Tetra-n-butyl titanate / kg 1 2 3 Acetic acid / kg 1.5 1 0.8 Water / kg 10 12 15 Stirring speed / (r / min) 4000 4500 5000 Stirring time / min 20 30 50

[0063] Example

[0064] Example 1, a silk finishing liquid, using raw materials as shown in Table 3, and its preparation process is as follows: a microcapsule mixture, an adhesive, a cross-linking agent, water and an organic acid are mixed at 20°C and a stirring speed of 500 r / min for 20 minutes to prepare a silk finishing liquid.

[0065] Example 2-4 is a silk finishing liquid, which differs from Example 1 in that the types and weights of the raw materials used are different, and the mixing conditions are different, as shown in Table 3.

[0066] Table 3 List of raw material types, weight settings and mixing conditions of silk finishing liquid in Examples 1-4

[0067]

[0068]

[0069] Example 5, a silk finishing liquid, differs from Example 1 in that propyltriacetoxysilane is substituted for methyltrimethoxysilane in equal amounts.

[0070] Example 6, a silk finishing liquid, differs from Example 1 in that 3-aminopropyltriethoxysilane replaces methyltrimethoxysilane in equal amounts.

[0071] Example 7, a silk finishing liquid, differs from Example 1 in that vinyltributylanoximesilane replaces methyltrimethoxysilane in equal amounts, and water-based epoxy adhesive replaces water-based polyurethane in equal amounts.

[0072] Example 8, a silk finishing liquid, differs from Example 1 in that triethylamine replaces methyltrimethoxysilane in equal amounts.

[0073] Example 9, a silk finishing liquid, differs from Example 1 in that maleic anhydride replaces methyltrimethoxysilane in equal amounts.

[0074] Example 10, a silk finishing liquid, differs from Example 1 in that an equal amount of nano-titanium dioxide powder (particle size 5 nm) replaces the titanium dioxide hydrosol.

[0075] Example 11 is a silk finishing liquid, which differs from Example 1 in that no ultraviolet absorber is used.

[0076] Example 12 is a silk finishing liquid, which differs from Example 1 in that titanium dioxide hydrosol is not used.

[0077] Example 13, a silk finishing liquid, differs from Example 1 in that titanium dioxide hydrosol and ultraviolet absorber are not used.

[0078] Example 14, a silk finishing liquid, differs from Example 1 in that the microcapsule mixed liquid of Preparation Example 4 is used.

[0079] Example 15, a silk finishing liquid, differs from Example 1 in that the microcapsule mixture adopts the composition of Preparation Example 5 and Preparation Example 6 in a mass ratio of 2:1.

[0080] Example 16, a silk finishing liquid, differs from Example 1 in that the microcapsule mixture adopts the composition of Preparation Example 5 and Preparation Example 6 in a mass ratio of 1:1.

[0081] Example 17, a silk finishing liquid, differs from Example 1 in that the microcapsule mixture adopts the composition of Preparation Example 5 and Preparation Example 6 in a mass ratio of 1:2.

[0082] Example 18, a method for treating a silk finishing liquid, using the following treatment process:

[0083] Silk fabric (weight 92 g / m2) was dried and rolled at 90°C, and then immersed in a silk finishing liquid (using Example 1) with a temperature of 20°C, a bath ratio of 1:8, and an immersion time of 30 min.

[0084] After impregnation, the fabric was tentered and then dried at 130° C. for 1 minute to prepare a silk fabric.

[0085] Example 19, a method for treating a silk finishing liquid, using the following treatment process:

[0086] The silk fabric (weight 92 g / m2) was dried and rolled at 100°C, and then immersed in a silk finishing liquid (using Example 2) with a temperature of 25°C, a bath ratio of 1:7, and an immersion time of 35 min.

[0087] After impregnation, the fabric was tentered and then dried at 120° C. for 1.5 minutes to prepare a silk fabric.

[0088] Example 20, a method for treating silk finishing liquid, using the following treatment process:

[0089] Silk fabric (weight 92 g / m2) was dried and rolled at 110°C, and then immersed in a silk finishing liquid (using Example 3) with a temperature of 30°C, a bath ratio of 1:6, and an immersion time of 40 min.

[0090] After impregnation, the fabric was tentered and then dried at 110° C. for 2 minutes to prepare a silk fabric.

[0091] Examples 21-34 are a method for treating a silk finishing liquid, which differs from Example 18 in that the silk finishing liquid is sequentially treated with the silk finishing of Examples 4-17.

[0092] Comparative Example

[0093] Comparative Example 1 is a silk finishing liquid, which differs from Example 4 in that no mesoporous material is used in the microcapsule mixture.

[0094] Comparative Example 2 is a silk finishing liquid, which differs from Example 4 in that no mesoporous material and cross-linking agent are used in the microcapsule mixture.

[0095] Comparative Example 3 is a silk finishing liquid, which differs from Example 4 in that no mesoporous material is used in the microcapsule mixture, and an equal amount of water-based epoxy adhesive is used instead of the water-based polyurethane adhesive.

[0096] Comparative Example 4 is a silk finishing liquid, which differs from Example 4 in that, in the microcapsule mixture, an emulsifier is used to replace dimethylolpropionic acid in an equal amount, and an aqueous epoxy adhesive is used to replace the aqueous polyurethane adhesive in an equal amount.

[0097] Comparative Examples 5-8 are a method for treating a silk finishing liquid. The difference from Example 30 is that the silk finishing liquids used are the silk finishing liquids of Comparative Examples 1-4, respectively.

[0098] Comparative Example 9, a method for treating a silk finishing liquid, differs from Example 22 in that no mesoporous material is used in the microcapsule mixture; in the silk finishing liquid, an equal amount of water-based epoxy adhesive is used instead of the water-based polyurethane adhesive, and an equal amount of triethylamine is used instead of the silane cross-linking agent methyltrimethoxysilane; and in the silk finishing liquid, no titanium dioxide hydrosol and no ultraviolet absorber are used.

[0099] Comparative Example 10, a method for treating a silk finishing liquid, differs from Example 33 in that no mesoporous material is used in the microcapsule mixture; in the silk finishing liquid, an equal amount of water-based epoxy adhesive is used instead of the water-based polyurethane adhesive, and an equal amount of triethylamine is used instead of the silane cross-linking agent methyltrimethoxysilane; and in the silk finishing liquid, no titanium dioxide hydrosol and no ultraviolet absorber are used.

[0100] Performance testing

[0101] Test 1: Moisturizing effect

[0102] Evaluation of moisturizing effect: The test samples were further processed into identical underwear and provided to 10 testers who had received skin feel evaluation training. The testers wore the identical underwear made from the test samples in turn and scored the moisturizing effect based on the skin feeling after wearing it, and the average value was taken.

[0103] The test standard uses a 1-10 scale, with the average score of 10 testers used to evaluate the effect. Among them, 1-3 points represent unsatisfactory (excluding 3), 3-5 points represent relatively satisfied (excluding 5), 5-7 points represent relatively satisfied (excluding 7), 7-9 points represent satisfied (excluding 9), and 9-10 points represent very satisfied.

[0104] Test 2: Washing resistance of moisturizing effect

[0105] Reference standard GBT8629-2017 Household washing and drying procedures for textile testing.

[0106] Detergent: Hengyuanxiang, Silver Silk Wool Silk Detergent, 300mL / bottle;

[0107] Rinsing equipment: Haier pulsator washing machine XQB100-Z206

[0108] The steps for each wash are as follows:

[0109] The test samples were further processed into the same underwear and put into a washing machine for washing. The concentration of detergent in the washing process was 5 ml / L.

[0110] Washing process: soak the clothes in the same detergent and rinse for 5 minutes; take out the underwear and rinse with clean water for 5 minutes each time, changing the water after each rinse, for a total of three rinses; take out the underwear and put it in the clothes drying basket, dry it at room temperature, away from light, and flatten it to dry. The above steps are for one wash;

[0111] After rinsing 20 times, 60 times, and 100 times, the underwear was placed at a temperature of 25°C and a humidity of 60% for 24 hours, and then the moisturizing effect of the silk fabric after washing was evaluated according to the evaluation method of Experiment 1.

[0112] Test samples: The silk fabrics prepared by the treatment method of the silk finishing liquid of Examples 18-34 were used as example samples; the silk fabrics prepared by the treatment method of the silk finishing liquid of Comparative Examples 5-10 were used as comparative samples.

[0113] Experimental results: The evaluation results of the moisturizing effect and the washability of the moisturizing effect of the silk fabrics prepared by Examples 18-34 and Comparative Examples 5-10 are shown in Table 4.

[0114] Table 4 Evaluation results of moisturizing effect and washability of silk fabrics prepared by the silk finishing liquid treatment methods of Examples 18-34 and Comparative Examples 5-10

[0115]

[0116]

[0117] Combining Examples 18-34 with Comparative Examples 5-10 and Table 4, it can be seen that:

[0118] Compared with comparative examples 5-10, the silk fabrics prepared in examples 18-34 have better moisturizing effect and water-resistant performance.

[0119] This may be because the wall material of the microcapsules used in Examples 18-34 is polyurethane, and mesoporous material is added to the polyurethane, which enhances the strength of the polyurethane wall material and reduces the rupture of the microcapsules during the washing and wearing processes of the silk fabric; at the same time, the skin care oil in the microcapsules is slowly released through the mesoporous material, thereby improving the moisturizing effect of the finished silk fabric and the washability of the skin care oil in the silk fabric.

[0120] Furthermore, by preferably using a silane crosslinking agent and / or adding an ultraviolet absorber UV531 and titanium dioxide hydrosol to the silk finishing liquid, the moisturizing effect of the silk fabric and the washability of the moisturizing effect are further improved.

[0121] Compared with Examples 25-26, the silk fabrics prepared in Examples 18 and 22-24 are softer and have better moisturizing effect and water-washing resistance.

[0122] This may be because the silk finishing liquid used in Examples 18 and Examples 22-24 uses a silicone cross-linking agent, which makes it easier for the chain segments of the film layer formed by the silk finishing liquid to move, making it easier for the skin care oil slowly released from the microcapsules to be transferred and evenly distributed on the surface of the silk fabric. The microcapsules slowly release more moisturizing oil, thereby making the silk fabric have a better moisturizing effect. Because the silk fabric using the silicone cross-linking agent is softer, the microcapsules bonded by the adhesive are not easy to break during the washing process, thereby making the silk fabric have better moisturizing performance and water resistance.

[0123] Compared with Example 18 and Example 22, the moisturizing performance and wash resistance of the silk fabrics prepared in Examples 23-24 were reduced.

[0124] This may be because the silane crosslinker used in the silk finishing liquid used in Example 23 contains more amino groups, and the silane crosslinker used in the silk finishing liquid used in Example 24 contains vinyl groups and a water-based epoxy adhesive is used; the use of amino groups with high polarity and ethoxy groups with large polarity and large molecular groups in the silane crosslinker may limit the rotation of the siloxy groups of the crosslinker and the movement of the molecular chain segments of the polyurethane, resulting in a decrease in the softness of the silk, and the silk fabric is easily scratched and the microcapsules are ruptured during the washing process; the interaction between the film layers formed by the silk finishing liquid is enhanced and / or the film layer formed by the water-based epoxy adhesive has a poor effect on the drainage of moisturizing oil, which leads to a decrease in the moisturizing performance of the silk fabric and the water-washing resistance of the moisturizing performance.

[0125] Compared with Comparative Example 9, the moisturizing effect and wash resistance of the silk fabrics prepared in Examples 18-19 and Example 22 are better than those in Comparative Example 9.

[0126] This may be because in Examples 18-19 and Example 22, mesoporous materials are used in the microcapsule mixture to enhance the sustained-release effect of the microcapsules on the moisturizing oil; aqueous polyurethane adhesives and silane crosslinkers are used in the silk finishing liquid, so that the film layer formed by the silk finishing liquid has a better drainage effect on the moisturizing oil, promotes the sustained-release of the microcapsules on the moisturizing oil, and uniformly distributes the moisturizing oil on the silk fabric; further, the silane crosslinker is used to make the silk fabric have better softness, reduce the rupture of the microcapsules during washing, and thus make the prepared silk fabric have excellent moisturizing effect and water-resistant performance with moisturizing effect.

[0127] Compared with Example 18, the moisturizing performance and water washing resistance of the silk fabric prepared in Example 27 are reduced; this may be because nano titanium dioxide powder is used instead of titanium dioxide hydrosol in Example 27, and the dispersibility of titanium dioxide powder is poor, which reduces the strength of the film layer formed by the adhesive, thereby causing the moisturizing performance and water washing resistance to decrease.

[0128] It can be seen from Examples 28-30 and Example 18 that the moisturizing performance and wash resistance of the silk fabric prepared in Example 18 are better than those in Examples 28-30.

[0129] The results show that the combination of ultraviolet absorber and titanium dioxide hydrosol in silk finishing liquid has synergistic effects. Titanium dioxide hydrosol not only improves the dispersion performance of ultraviolet absorber, but also improves the strength of the adhesive film and the bonding strength with silk fabric, making the silk fabric have excellent moisturizing performance and water resistance.

[0130] Compared with Example 18, the moisturizing effect of the silk fabric prepared in Example 31 was reduced. This may be because the wall material of the microcapsules in the microcapsule mixture in Example 31 used polyethylene glycol 1500 in an equal amount to replace the hydroxyl-terminated polydimethylsiloxane, which reduced the rotation or mobility of the soft segments of the microcapsule wall material. This reduced the amount of moisturizing oil in the microcapsules that was slowly released through the wall material, resulting in a reduced moisturizing effect of the prepared silk fabric.

[0131] Compared with Examples 18-31, the silk fabrics prepared in Examples 32-34 exhibited superior moisturizing properties. This may be because the emollient vitamin E and aloe vera oil contained in the microcapsules in Examples 32-34 were separately microcapsuled, which enhanced the sustained release of vitamin E and aloe vera oil, thereby improving the moisturizing properties of the resulting silk fabrics.

[0132] Compared with Comparative Example 10, the silk fabrics prepared in Examples 32-34 have better moisturizing effect and water resistance of moisturizing effect.

[0133] This may be because in Examples 32-34, mesoporous materials are used in the microcapsule mixture to enhance the sustained-release effect of the microcapsules on the moisturizing oil; water-based polyurethane adhesive and silane cross-linking agent are used in the silk finishing liquid, and the film layer formed by the adhesive has a good drainage effect on the moisturizing oil sustained-released by the microcapsules, further promoting the sustained-release of the moisturizing oil by the microcapsules and the uniform distribution of the moisturizing oil on the silk fabric; the use of silane cross-linking agent makes the silk fabric have better softness, reduces the rupture of microcapsules during washing, and thus makes the silk fabric have excellent moisturizing effect and water-resistant performance with moisturizing effect.

[0134] Test 3: Yellowing resistance

[0135] Using UVA (340) lamp as the light source, the test sample was placed in a fluorescent UV aging machine for continuous illumination for 168 hours; the test conditions were: temperature (60±3)℃, irradiance 0.68W / m 2 , dry without condensation; take it out after the illumination is over, compare it with the test sample that has not been illuminated, and measure the color change with a colorimeter. The unit of color change value is △E. The smaller the measured value, the better the yellowing resistance.

[0136] Test 4: Softness and gloss

[0137] Simulating the factory inspection process, the system uses the manual inspection method of factory inspectors to evaluate the changes in the gloss and softness of the fabric through touch and visual observation.

[0138] The inspection method is as follows:

[0139] Employees with more than two years of inspection experience are selected to compare and rate test samples and comparison fabric samples (samples not treated with silk finishing fluid).

[0140] Each roll of fabric is randomly inspected 10 times, with an area of ​​30×30 cm as the unit inspection area for each inspection. The gloss and softness of the inspected samples are compared with those of the untreated original silk fabric samples, and the average score is taken. The scoring criteria are as follows:

[0141] 1 point: The gloss and soft feel are obviously inferior to the original silk fabric, which has a significant impact on sales. The fabric cannot be sold even after being downgraded.

[0142] 1-2 points (excluding 2): The gloss and soft feel are not as good as the original silk fabric, and the fabric can be sold after being downgraded.

[0143] 2-3 points (excluding 3): The gloss and softness are slightly inferior to the original silk fabric, but there is no need to downgrade.

[0144] 3-4 points: The gloss and soft feel are similar to the original silk fabric and no downgrading is required.

[0145] Test samples: The silk fabrics prepared by the treatment method of the silk finishing liquid of Examples 18-34 were used as example samples; the silk fabrics prepared by the treatment method of the silk finishing liquid of Comparative Examples 7-10 were used as comparative samples.

[0146] Experimental results: The evaluation results of yellowing resistance, softness and gloss of the silk fabrics prepared by the treatment methods of the silk finishing liquids of Examples 18-34 and Comparative Examples 7-10 are shown in Table 5.

[0147] Table 5 Evaluation results of yellowing resistance, softness and gloss of silk fabrics prepared by the silk finishing liquid treatment methods of Examples 18-34 and Comparative Examples 7-10

[0148]

[0149]

[0150] Combining Examples 18-34 with Comparative Examples 7-10 and Table 5, it can be seen that:

[0151] Compared with comparative examples 7-10, the silk fabrics prepared in Examples 18-34 have better gloss, feel and yellowing resistance than those in comparative examples 7-10.

[0152] This may be because the aqueous polyurethane and / or titanium dioxide hydrosol and the ultraviolet absorber are used in combination in Examples 18-34, so that the prepared silk fabrics have better gloss, feel and yellowing resistance.

[0153] In Comparative Examples 7-10, the use of a water-based epoxy adhesive that is easily oxidized and discolored, and the absence of titanium dioxide hydrosol and ultraviolet absorber, resulted in poor yellowing resistance and glossiness of the film layer formed by the adhesive.

[0154] The addition of an emulsifier to the adhesive in Comparative Example 8 caused the glossiness of the film formed by the adhesive to decrease significantly.

[0155] Compared with Examples 25-26, the silk fabrics prepared in Examples 18 and 22-24 are softer and have better color; this may be because the silk finishing liquid used in Examples 18 and 22-24 contains a silane crosslinking agent, which makes the finished silk softer and less damaged during washing. The silk fabric has better flatness after washing, and the silk fabric has better gloss.

[0156] Compared with Example 18 and Example 22, the silk fabrics prepared in Examples 23-24 have poor yellowing resistance and the softness and color of the silk fabrics are reduced. This may be because the silk finishing liquid used in Example 23 contains more polar group amino in the silane crosslinker, and the silk finishing liquid used in Example 24 contains more active group vinyl in the silane crosslinker, and the water-based epoxy adhesive used makes the yellowing resistance and color of the prepared silk fabrics worse.

[0157] Compared with Comparative Example 9, the silk fabrics prepared in Examples 18-19 and Example 22 have better color and feel, indicating that the use of aqueous polyurethane adhesive, cross-linking agent methyltrimethoxysilane, titanium dioxide hydrosol and ultraviolet absorber in the microcapsule mixture makes the silk fabric more flexible and has better anti-wrinkle effect, thereby making the prepared silk fabric have better feel, color and yellowing resistance.

[0158] Compared with Example 18, the yellowing resistance and color of the silk fabric prepared in Example 27 are reduced; this may be because nano titanium dioxide powder is used instead of titanium dioxide hydrosol in Example 27, and the dispersibility of titanium dioxide powder is worse than that of titanium dioxide hydrosol, causing more diffuse reflection of light on the silk surface, resulting in a reduction in the yellowing resistance and color of the silk fabric.

[0159] It can be seen from Examples 28-30 and Example 18 that the yellowing resistance of the silk fabric prepared in Example 18 is better than that of Examples 28-30; this indicates that the use of ultraviolet absorbers and titanium dioxide hydrosol in combination in the silk finishing liquid has a synergistic effect, and the titanium dioxide hydrosol not only improves the dispersion performance of the ultraviolet absorber, but also improves the strength of the film formed by the adhesive, so that the prepared silk fabric has excellent yellowing resistance.

[0160] Compared with Comparative Example 10, the silk fabrics prepared in Examples 32-34 have better color and feel.

[0161] It shows that the silane crosslinker and water-based polyurethane in Examples 32-34 are beneficial to maintaining the softness of silk fabrics and improving the anti-wrinkle effect, so that the silk fabrics have good color and feel.

[0162] This specific embodiment is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make non-creative modifications to the present embodiment as needed, but as long as they are within the scope of the claims of the present application, they are protected by the patent law.

Claims

1. A silk finishing liquid, characterized in that: The composition comprises, by weight, 15-30 parts of a microcapsule mixture, 10-30 parts of a binder, 2-5 parts of a silane crosslinking agent, 30-40 parts of water, 0.4-0.8 parts of an organic acid catalyst, 1-4 parts of an ultraviolet absorber, and 3-8 parts of a titanium dioxide hydrosol. The silane crosslinking agent is one of dodecyltriethoxysilane, methyltrimethoxysilane, propyltriacetoxysilane and propyltriacetoxysilane; The adhesive is water-based polyurethane; The microcapsule mixture is a mixture containing microcapsules with skin care oil as the core material and polyurethane as the wall material; wherein the raw materials of the microcapsule mixture include 120-150 parts by mass of skin care oil, 10-20 parts by mass of mesoporous material, 100-150 parts by mass of polyether diol, 100-110 parts by mass of diisocyanate, 0.1-0.2 parts by mass of catalyst, 6-10 parts by mass of glycerol, 6-15 parts by mass of dimethylolpropionic acid, 2-5 parts by mass of triethylamine, 3-8 parts by mass of ethylenediamine, 8-15 parts by mass of acetone, 30-60 parts by mass of hydroxy-terminated polydimethylsiloxane and 800 parts by mass of water; The mesoporous material is one of mesoporous silica, nano zeolite and nano bentonite; The preparation process of the microcapsule mixture is as follows: Preparation of polyurethane prepolymer: polyether diol, hydroxyl-terminated polydimethylsiloxane, mesoporous material and glycerol are mixed to form a mixed solution, the mixed solution is heated to 70-90°C, diphenylmethane diisocyanate is added under nitrogen protection and stirring at 300-500 rpm, and the reaction is carried out for 0.6-1.2 hours to prepare a polyurethane prepolymer; Salt formation and emulsification: After adding dimethylolpropionic acid to the polyurethane prepolymer, react under stirring for 2.5 hours; then cool and add acetone; then add skin care oil and triethylamine, react under stirring at 3000-5000 r / min for 1 hour, cool and add water at 5000-8000 r / min for emulsification; then add ethylenediamine for chain extension, raise the temperature to 70-90°C, and react under stirring at 500-700 r / min for 0.5-1 hour to prepare a microcapsule mixture.

2. A silk finishing liquid according to claim 1, characterized in that The skin care oil is at least one of olive oil, aloe vera oil, vitamin E and vitamin C.

3. A silk finishing liquid according to claim 1, characterized in that The titanium dioxide hydrosol is a mixed solution prepared by reacting 1-3 parts by mass of n-butyl titanate and 10-15 parts by mass of water under the catalysis of acetic acid.

4. A method for treating silk using the silk finishing liquid according to any one of claims 1 to 3, characterized in that: The steps include: The microcapsule mixture, adhesive, cross-linking agent, water and organic acid are mixed to prepare a silk finishing solution; The silk fabric is dried, rolled, and then impregnated with silk finishing liquid; The padded silk fabric is tentered and then hot-air finished at 110-130° C. for 1-2 minutes to prepare the silk fabric.

5. The method for treating silk finishing liquid according to claim 4, characterized in that: The silk fabric is immersed in the silk finishing liquid for 30-40 minutes; the temperature of the silk finishing liquid during the immersion is 20-30°C.

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