A soft and fluffy treatment agent for non-woven fabrics and preparation method thereof

A nonwoven fabric soft and fluffy treatment agent was prepared by reacting nano-silica with silane coupling agent and vegetable oil, which solved the problems of reduced nonwoven fabric thickness and yellowing, and improved the hydrophilicity, fluffiness and mechanical properties of the fabric.

CN118773912BActive Publication Date: 2025-01-07GUANGZHOU TORUI TECH CO LTD
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Patent Information

Application Number
CN202411055025.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-08-02
Publication Date
2025-01-07
Estimated Expiration
2044-08-02

AI Technical Summary

Technical Problem

Existing nonwoven fabrics have reduced thickness after softening treatment, affecting hydrophilicity and mechanical properties, and silicone treatment causes fabric pilling and yellowing problems.

Method used

A nonwoven fabric soft and fluffy treatment agent was prepared by modifying the surface of nano-silica with aminosilane and reacting it with dimethylolpropionic acid hyperbranching, combined with silane coupling agent, vegetable oil and diethylenetriamine. The agent improves the fabric properties through hydrogen bonding and oil structure.

Benefits of technology

It improves the hydrophilicity, bulkiness, and mechanical properties of nonwoven fabrics, prevents yellowing of the fabric, enhances the skin-friendly and smooth feel, and is environmentally friendly.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention proposes a non-woven fabric soft and fluffy treatment agent and a preparation method thereof, and belongs to the technical field of non-woven fabrics. The surface of nano silicon dioxide is modified with aminosilane and then subjected to hyperbranching reaction with dimethylol propionic acid, further modified with a silane coupling agent, reacted with the reaction product of vegetable oil and diethylenetriamine, and then mixed with glycerol, water, Tween-80, and aminosilicone oil, and emulsified to obtain a non-woven fabric soft and fluffy treatment agent. The non-woven fabric soft and fluffy treatment agent prepared by the present invention has good hydrophilicity and fluffiness, and is green and environmentally friendly, improves the whiteness of the product, avoids yellowing of the fabric and phenol yellowing, and can improve the mechanical properties of the product to a certain extent, improve the skin-friendly feel and smoothness of the fabric, and has broad application prospects.
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Description

Technical Field

[0001] The invention relates to the technical field of non-woven fabrics, and in particular to a soft and fluffy treatment agent for non-woven fabrics and a preparation method thereof. Background Art

[0002] At present, after non-woven fabrics are softened in the market, the thickness of non-woven fabrics is reduced by about 13% compared with before due to the increase of moisture in the production process and the stretching of winding. After the thickness is reduced, the relative packaging thickness will also be reduced, which gives consumers a bad feeling. In addition, some non-woven fabrics are very tightly compressed during the production process and are not thick enough. Silicone is currently used in the market to increase the softness and thickness of finished fiber products, but in actual applications, fabrics treated with silicone will affect their hydrophilicity and mechanical properties to a certain extent, increase the fuzziness of the fabric surface, and also cause yellowing and phenolic yellowing of the fabric. Summary of the invention

[0003] The purpose of the present invention is to provide a non-woven fabric soft and fluffy treatment agent and a preparation method thereof, which is hydrophilic, fluffy, green and environmentally friendly, improves the whiteness of the product, avoids yellowing and phenolic yellowing of the fabric, and can improve the mechanical properties of the product to a certain extent, improve the skin-friendly and smooth feel of the fabric, and has broad application prospects.

[0004] The technical solution of the present invention is achieved in this way:

[0005] The invention provides a method for preparing a non-woven fabric soft and fluffy treatment agent. The surface of nano silicon dioxide is modified with aminosilane, and then subjected to hyperbranching reaction with dimethylol propionic acid, further modified with a silane coupling agent, reacted with a reaction product of vegetable oil and diethylenetriamine, and then uniformly mixed with glycerol, water, Tween-80 and amino silicone oil, and emulsified to prepare the non-woven fabric soft and fluffy treatment agent.

[0006] As a further improvement of the present invention, the following steps are included:

[0007] S1. Preparation of amino-modified nano-silica: adding nano-silica and aminosilane to ethanol, heating and stirring to react, centrifuging, washing, and drying to obtain amino-modified nano-silica;

[0008] S2. Preparation of hyperbranched nano-silica: adding amino-modified nano-silica to toluene, adding dimethylol propionic acid and p-toluenesulfonic acid, heating under reflux with stirring, centrifuging, washing, and drying to obtain hyperbranched nano-silica;

[0009] S3. Preparation of silane coupling agent modified nano-silica: adding the composite silane coupling agent to ethanol, adding hyperbranched nano-silica, heating and stirring the reaction, centrifuging, washing, and drying to obtain modified nano-silica;

[0010] S4. Preparation of intermediate: Mix vegetable oil and diethylenetriamine, heat and stir to react, add modified nano-silica, stir to react at room temperature, centrifuge, wash, and dry to obtain an intermediate;

[0011] S5. Preparation of a soft and fluffy treatment agent for non-woven fabrics: glycerin, water, Tween-80, amino silicone oil and an intermediate are uniformly mixed and emulsified to prepare a soft and fluffy treatment agent for non-woven fabrics.

[0012] As a further improvement of the present invention, the mass ratio of the nano-silica and the aminosilane in step S1 is 10:2-3, the average particle size of the nano-silica is 80-150nm, the temperature of the heating and stirring reaction is 40-50°C, the time is 1-3h, and the aminosilane is selected from at least one of γ-aminopropyltrimethoxysilane, γ-aminopropyltriethoxysilane, N-β (aminoethyl)-γ-aminopropyltrimethoxysilane, N-β (aminoethyl)-γ-aminopropyltriethoxysilane, N-β (aminoethyl)-γ-aminopropylmethyldimethoxysilane, N-β (aminoethyl)-γ-aminopropylmethyldiethoxysilane, and diethylenetriaminopropyltrimethoxysilane.

[0013] As a further improvement of the present invention, in step S2, the mass ratio of amino-modified nano-silica, dimethylolpropionic acid and p-toluenesulfonic acid is 5-7:22-24:0.1-0.2, and the heating reflux stirring reaction time is 4-6h.

[0014] As a further improvement of the present invention, the mass ratio of the composite silane coupling agent and the hyperbranched nano-silica in step S3 is 2-3:10-12, the temperature of the heating and stirring reaction is 45-55°C, the time is 1-3h, and the composite silane coupling agent is a mixture of KH550 and KH560, and the mass ratio is 3-5:10.

[0015] As a further improvement of the present invention, the mass ratio of the vegetable oil, diethylenetriamine and modified nano-silicon dioxide in step S4 is 10:4-7:25-30, the temperature of the heating and stirring reaction is 135-145°C, the time is 4-5h, the time of the room temperature stirring reaction is 2-4h, and the vegetable oil is selected from at least one of soybean oil, peanut oil, sesame oil, rapeseed oil, linseed oil and corn oil.

[0016] As a further improvement of the present invention, the mass ratio of glycerol, water, Tween-80, amino silicone oil and intermediate in step S5 is 20-30:10-20:2-3:3-5:10-12, and the emulsification conditions are 7000-8000 r / min for 10-20 min.

[0017] As a further improvement of the present invention, the present invention specifically comprises the following steps:

[0018] S1. Preparation of amino-modified nano-silica: 10 parts by weight of nano-silica and 2-3 parts by weight of aminosilane were added to ethanol, heated to 40-50°C, stirred for reaction for 1-3h, centrifuged, washed, and dried to obtain amino-modified nano-silica;

[0019] S2. Preparation of hyperbranched nano-silica: 5-7 parts by weight of amino-modified nano-silica was added to toluene, 22-24 parts by weight of dimethylol propionic acid and 0.1-0.2 parts by weight of p-toluenesulfonic acid were added, the reaction was stirred under reflux for 4-6h, centrifuged, washed and dried to obtain hyperbranched nano-silica;

[0020] S3. Preparation of silane coupling agent modified nano-silica: 2-3 parts by weight of the composite silane coupling agent was added to ethanol, 10-12 parts by weight of hyperbranched nano-silica was added, heated to 45-55 ° C, stirred for 1-3h, centrifuged, washed, and dried to obtain modified nano-silica;

[0021] The composite silane coupling agent is a mixture of KH550 and KH560, with a mass ratio of 3-5:10;

[0022] S4. Preparation of intermediate: 10 parts by weight of vegetable oil and 4-7 parts by weight of diethylenetriamine were mixed, heated to 135-145 ° C, stirred for 4-5h, added 25-30 parts by weight of modified nano-silica, stirred at room temperature for 2-4h, centrifuged, washed, and dried to obtain an intermediate;

[0023] S5. Preparation of a soft and fluffy treatment agent for non-woven fabrics: 20-30 parts by weight of glycerol, 10-20 parts by weight of water, 2-3 parts by weight of Tween-80, 3-5 parts by weight of amino silicone oil and 10-12 parts by weight of the intermediate are mixed evenly, and emulsified at 7000-8000 r / min for 10-20 min to obtain a soft and fluffy treatment agent for non-woven fabrics.

[0024] The present invention further protects a non-woven fabric soft and fluffy treating agent prepared by the above preparation method.

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

[0026] The present invention uses inorganic nano-silicon dioxide as rigid particles, firstly performs aminosilane modification on the surface, and then carries out amino groups on the surface, and the amino groups react with dimethylol propionic acid monomers to form hyperbranched hydroxy nano-silicon dioxide with rich hydroxyl structures. On the one hand, the hydroxyl structures can subsequently form hydrogen bonds with KH550 in the composite silane coupling agent, and on the other hand, the polyhydroxyl structures also improve the hydrophilicity of the fabric. Using inorganic nano-silicon dioxide as rigid particles also greatly improves the mechanical properties of the fabric, and improves its whiteness, and avoids yellowing and phenol yellowing of the fabric.

[0027] Vegetable oil is rich in fat, cholesterol-free, unsaturated fatty acids, and rich in vitamin A, vitamin B, and vitamin E, which can effectively repair wounds or rough skin. After reacting with diethylenetriamine, the secondary amino group on the product reacts and couples with the epoxy group of modified nano-silicon dioxide to obtain an intermediate, which is biodegradable, improves the environmental friendliness of the product, and also improves the fluffiness of the fabric. It not only has the same silane chain structure as organic silane, but also forms a continuous organic silicon film on the surface of the fabric. The bond angle of the silicon-oxygen bond can be stretched and retracted under the action of external force, which improves the smoothness of the finished product. In addition, the orderly arrangement of organic silicon molecules on the fiber also gives the fabric a fluffy feel.

[0028] The non-woven fabric soft and fluffy treatment agent prepared by the invention has good hydrophilicity and fluffyness, is green and environmentally friendly, improves the whiteness of the product, avoids yellowing and phenolic yellowing of the fabric, can improve the mechanical properties of the product to a certain extent, and improves the skin-friendly feel and smoothness of the fabric, and has broad application prospects. DETAILED DESCRIPTION

[0029] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0030] Nano-silicon dioxide, with an average particle size of 100 nm, was purchased from Hubei Huifu Nanomaterials Co., Ltd.

[0031] Amino silicone oil, pH = 5.5-6.5, active ingredient content > 60%, purchased from Shandong Huachen New Materials Co., Ltd.

[0032] Example 1

[0033] This embodiment provides a method for preparing a soft and fluffy treatment agent for non-woven fabrics, which specifically comprises the following steps:

[0034] S1. Preparation of amino-modified nano-silica: 10 g of nano-silica and 2 g of N-β (aminoethyl) -γ-aminopropylmethyldimethoxysilane were added to 200 mL of ethanol, heated to 40° C., stirred for reaction for 1 h, centrifuged, washed, and dried to obtain amino-modified nano-silica;

[0035] S2. Preparation of hyperbranched nano-silica: 5 g of amino-modified nano-silica was added to 500 mL of toluene, 22 g of dimethylol propionic acid and 0.1 g of p-toluenesulfonic acid were added, the reaction was heated under reflux with stirring for 4 h, centrifuged, washed, and dried to obtain hyperbranched nano-silica;

[0036] S3. Preparation of silane coupling agent modified nano-silica: 2 g of composite silane coupling agent was added to 200 mL of ethanol, 10 g of hyperbranched nano-silica was added, heated to 45 ° C, stirred for 1 h, centrifuged, washed, and dried to obtain modified nano-silica;

[0037] The composite silane coupling agent is a mixture of KH550 and KH560, with a mass ratio of 3:10;

[0038] S4. Preparation of intermediate: 10 g of soybean oil and 4 g of diethylenetriamine were mixed, heated to 135 ° C, stirred for 4 h, 25 g of modified nano-silica was added, stirred for 2 h at room temperature, centrifuged, washed, and dried to obtain an intermediate;

[0039] S5. Preparation of a soft and fluffy treatment agent for non-woven fabrics: 20 g of glycerol, 10 mL of water, 2 g of Tween-80, 3 g of amino silicone oil and 10 g of the intermediate were mixed evenly, and emulsified at 7000 r / min for 10 min to obtain a soft and fluffy treatment agent for non-woven fabrics.

[0040] Example 2

[0041] This embodiment provides a method for preparing a soft and fluffy treatment agent for non-woven fabrics, which specifically comprises the following steps:

[0042] S1. Preparation of amino-modified nano-silica: 10 g of nano-silica and 3 g of γ-aminopropyltrimethoxysilane were added to 200 mL of ethanol, heated to 50° C., stirred for reaction for 3 h, centrifuged, washed, and dried to obtain amino-modified nano-silica;

[0043] S2. Preparation of hyperbranched nano-silica: 7 g of amino-modified nano-silica was added to 500 mL of toluene, 24 g of dimethylol propionic acid and 0.2 g of p-toluenesulfonic acid were added, the reaction was stirred under reflux for 6 h, centrifuged, washed, and dried to obtain hyperbranched nano-silica;

[0044] S3. Preparation of silane coupling agent modified nano-silica: 3 g of composite silane coupling agent was added to 200 mL of ethanol, 12 g of hyperbranched nano-silica was added, heated to 55 ° C, stirred for 3 h, centrifuged, washed, and dried to obtain modified nano-silica;

[0045] The composite silane coupling agent is a mixture of KH550 and KH560, with a mass ratio of 5:10;

[0046] S4. Preparation of intermediate: 10 g of sesame oil and 7 g of diethylenetriamine were mixed, heated to 145 ° C, stirred for 5 h, 30 g of modified nano-silica was added, stirred for 4 h at room temperature, centrifuged, washed, and dried to obtain an intermediate;

[0047] S5. Preparation of a soft and fluffy treatment agent for non-woven fabrics: 30 g of glycerol, 20 mL of water, 3 g of Tween-80, 5 g of amino silicone oil and 12 g of the intermediate were mixed evenly, and emulsified at 8000 r / min for 20 min to obtain a soft and fluffy treatment agent for non-woven fabrics.

[0048] Example 3

[0049] This embodiment provides a method for preparing a soft and fluffy treatment agent for non-woven fabrics, which specifically comprises the following steps:

[0050] S1. Preparation of amino-modified nano-silica: 10 g of nano-silica and 2.5 g of N-β (aminoethyl) -γ-aminopropyltrimethoxysilane were added to 200 mL of ethanol, heated to 450 ° C, stirred for 2 h, centrifuged, washed, and dried to obtain amino-modified nano-silica;

[0051] S2. Preparation of hyperbranched nano-silica: 6 g of amino-modified nano-silica was added to 500 mL of toluene, 23 g of dimethylol propionic acid and 0.15 g of p-toluenesulfonic acid were added, the reaction was heated under reflux with stirring for 5 h, centrifuged, washed, and dried to obtain hyperbranched nano-silica;

[0052] S3. Preparation of silane coupling agent modified nano-silica: 2.5 g of composite silane coupling agent was added to 200 mL of ethanol, 11 g of hyperbranched nano-silica was added, heated to 50 ° C, stirred for 2 h, centrifuged, washed, and dried to obtain modified nano-silica;

[0053] The composite silane coupling agent is a mixture of KH550 and KH560, with a mass ratio of 4:10;

[0054] S4. Preparation of intermediate: 10 g corn oil and 5.5 g diethylenetriamine were mixed, heated to 140 ° C, stirred for 4.5 h, 27 g modified nano-silica was added, stirred for 3 h at room temperature, centrifuged, washed, and dried to obtain an intermediate;

[0055] S5. Preparation of a soft and fluffy treatment agent for non-woven fabrics: 25 g of glycerol, 15 mL of water, 2.5 g of Tween-80, 4 g of amino silicone oil and 11 g of the intermediate were mixed evenly, and emulsified at 7500 r / min for 15 min to obtain a soft and fluffy treatment agent for non-woven fabrics.

[0056] Example 4

[0057] Compared with Example 3, the difference is that the composite silane coupling agent is replaced by a single KH550.

[0058] The details are as follows:

[0059] S1. Preparation of amino-modified nano-silica: 10 g of nano-silica and 2.5 g of N-β (aminoethyl) -γ-aminopropyltrimethoxysilane were added to 200 mL of ethanol, heated to 450 ° C, stirred for 2 h, centrifuged, washed, and dried to obtain amino-modified nano-silica;

[0060] S2. Preparation of hyperbranched nano-silica: 6 g of amino-modified nano-silica was added to 500 mL of toluene, 23 g of dimethylol propionic acid and 0.15 g of p-toluenesulfonic acid were added, the reaction was heated under reflux with stirring for 5 h, centrifuged, washed, and dried to obtain hyperbranched nano-silica;

[0061] S3. Preparation of silane coupling agent modified nano-silica: 2.5 g of silane coupling agent KH550 was added to 200 mL of ethanol, 11 g of hyperbranched nano-silica was added, heated to 50 ° C, stirred for 2 h, centrifuged, washed, and dried to obtain modified nano-silica;

[0062] S4. Preparation of intermediate: 10 g corn oil and 5.5 g diethylenetriamine were mixed, heated to 140 ° C, stirred for 4.5 h, 27 g modified nano-silica was added, stirred for 3 h at room temperature, centrifuged, washed, and dried to obtain an intermediate;

[0063] S5. Preparation of a soft and fluffy treatment agent for non-woven fabrics: 25 g of glycerol, 15 mL of water, 2.5 g of Tween-80, 4 g of amino silicone oil and 11 g of the intermediate were mixed evenly, and emulsified at 7500 r / min for 15 min to obtain a soft and fluffy treatment agent for non-woven fabrics.

[0064] Example 5

[0065] Compared with Example 3, the difference is that the composite silane coupling agent is replaced by a single KH560.

[0066] The details are as follows:

[0067] S1. Preparation of amino-modified nano-silica: 10 g of nano-silica and 2.5 g of N-β (aminoethyl) -γ-aminopropyltrimethoxysilane were added to 200 mL of ethanol, heated to 450 ° C, stirred for 2 h, centrifuged, washed, and dried to obtain amino-modified nano-silica;

[0068] S2. Preparation of hyperbranched nano-silica: 6 g of amino-modified nano-silica was added to 500 mL of toluene, 23 g of dimethylol propionic acid and 0.15 g of p-toluenesulfonic acid were added, the reaction was heated under reflux with stirring for 5 h, centrifuged, washed, and dried to obtain hyperbranched nano-silica;

[0069] S3. Preparation of silane coupling agent modified nano-silica: 2.5 g of silane coupling agent KH560 was added to 200 mL of ethanol, 11 g of hyperbranched nano-silica was added, heated to 50 ° C, stirred for 2 h, centrifuged, washed, and dried to obtain modified nano-silica;

[0070] S4. Preparation of intermediate: 10 g corn oil and 5.5 g diethylenetriamine were mixed, heated to 140 ° C, stirred for 4.5 h, 27 g modified nano-silica was added, stirred for 3 h at room temperature, centrifuged, washed, and dried to obtain an intermediate;

[0071] S5. Preparation of a soft and fluffy treatment agent for non-woven fabrics: 25 g of glycerol, 15 mL of water, 2.5 g of Tween-80, 4 g of amino silicone oil and 11 g of the intermediate were mixed evenly, and emulsified at 7500 r / min for 15 min to obtain a soft and fluffy treatment agent for non-woven fabrics.

[0072] Comparative Example 1

[0073] Compared with Example 3, the difference is that steps S1 and S2 are not performed.

[0074] The details are as follows:

[0075] S1. Preparation of silane coupling agent modified nano-silica: 2.5 g of composite silane coupling agent was added to 200 mL of ethanol, 11 g of nano-silica was added, the mixture was heated to 50° C., stirred for reaction for 2 h, centrifuged, washed, and dried to obtain modified nano-silica;

[0076] The composite silane coupling agent is a mixture of KH550 and KH560, with a mass ratio of 4:10;

[0077] S2. Preparation of intermediate: 10 g corn oil and 5.5 g diethylenetriamine were mixed, heated to 140 ° C, stirred for 4.5 h, 27 g modified nano-silica was added, stirred for 3 h at room temperature, centrifuged, washed, and dried to obtain an intermediate;

[0078] S3. Preparation of a soft and fluffy treatment agent for non-woven fabrics: 25 g of glycerol, 15 mL of water, 2.5 g of Tween-80, 4 g of amino silicone oil and 11 g of the intermediate were mixed evenly, and emulsified at 7500 r / min for 15 min to obtain a soft and fluffy treatment agent for non-woven fabrics.

[0079] Comparative Example 2

[0080] Compared with Example 3, the difference is that step S3 is not performed.

[0081] The details are as follows:

[0082] S1. Preparation of amino-modified nano-silica: 10 g of nano-silica and 2.5 g of N-β (aminoethyl) -γ-aminopropyltrimethoxysilane were added to 200 mL of ethanol, heated to 450 ° C, stirred for 2 h, centrifuged, washed, and dried to obtain amino-modified nano-silica;

[0083] S2. Preparation of hyperbranched nano-silica: 6 g of amino-modified nano-silica was added to 500 mL of toluene, 23 g of dimethylol propionic acid and 0.15 g of p-toluenesulfonic acid were added, the reaction was heated under reflux with stirring for 5 h, centrifuged, washed, and dried to obtain hyperbranched nano-silica;

[0084] S3. Preparation of intermediate: 10 g corn oil and 5.5 g diethylenetriamine were mixed, heated to 140 ° C, stirred for 4.5 h, 27 g hyperbranched nano-silica was added, stirred for 3 h at room temperature, centrifuged, washed, and dried to obtain an intermediate;

[0085] S4. Preparation of a soft and fluffy treatment agent for non-woven fabrics: 25 g of glycerol, 15 mL of water, 2.5 g of Tween-80, 4 g of amino silicone oil and 11 g of the intermediate were mixed evenly, and emulsified at 7500 r / min for 15 min to obtain a soft and fluffy treatment agent for non-woven fabrics.

[0086] Comparative Example 3

[0087] Compared with Example 3, the difference is that step S4 is not performed.

[0088] The details are as follows:

[0089] S1. Preparation of amino-modified nano-silica: 10 g of nano-silica and 2.5 g of N-β (aminoethyl) -γ-aminopropyltrimethoxysilane were added to 200 mL of ethanol, heated to 450 ° C, stirred for 2 h, centrifuged, washed, and dried to obtain amino-modified nano-silica;

[0090] S2. Preparation of hyperbranched nano-silica: 6 g of amino-modified nano-silica was added to 500 mL of toluene, 23 g of dimethylol propionic acid and 0.15 g of p-toluenesulfonic acid were added, the reaction was heated under reflux with stirring for 5 h, centrifuged, washed, and dried to obtain hyperbranched nano-silica;

[0091] S3. Preparation of silane coupling agent modified nano-silica: 2.5 g of composite silane coupling agent was added to 200 mL of ethanol, 11 g of hyperbranched nano-silica was added, heated to 50 ° C, stirred for 2 h, centrifuged, washed, and dried to obtain modified nano-silica;

[0092] The composite silane coupling agent is a mixture of KH550 and KH560, with a mass ratio of 4:10;

[0093] S4. Preparation of a soft and fluffy treatment agent for non-woven fabrics: 25 g of glycerol, 15 mL of water, 2.5 g of Tween-80, 4 g of amino silicone oil and 11 g of modified nano-silica were mixed evenly, and emulsified at 7500 r / min for 15 min to obtain a soft and fluffy treatment agent for non-woven fabrics.

[0094] Comparative Example 4

[0095] Compared with Example 3, the difference is that no intermediate is added in step S5.

[0096] The details are as follows:

[0097] Preparation of non-woven fabric soft and fluffy treatment agent: 25g glycerol, 15mL water, 2.5g Tween-80, and 15g amino silicone oil were mixed evenly, and emulsified at 7500r / min for 15min to prepare the non-woven fabric soft and fluffy treatment agent.

[0098] Test Example 1

[0099] Dilute the non-woven fabric fluffy treatment agent 50 times, spray it evenly on the surface of the non-woven fabric, bake at 105℃ for 5 minutes, and place it in a dry place for 24 hours. The treatment group that was not sprayed with the non-woven fabric fluffy treatment agent was used as the control.

[0100] (1) Textile water absorption test: The hydrophilic effect (water drop method) is carried out in accordance with the "Textile Water Absorption Test" (AATCC22-2010).

[0101] (2) Hand feel test: The test is conducted by touching the fabric with hands, mainly for softness, smoothness and fluffiness. The test is evaluated by more than 5 professionals. The hand feel is graded from 1 to 5, with 5 being the best and 1 being the worst.

[0102] (3) Whiteness test: The whiteness test of textile fibers was carried out in accordance with the Test Method for Whiteness of Textile Fibers (GB / T17644-2008).

[0103] (4) Fluffiness test: 40 sheets of nonwoven fabric were stacked and the thickness before and after spraying was measured using a micrometer.

[0104] (5) Strength retention rate test: According to GB / T 19976-2005 "Test of bursting strength of textiles - Steel ball method", the fabric strength was measured on a YG031D electronic bursting strength tester, and the strength retention rate (%) was calculated.

[0105] Strength retention rate (%) = sample tissue strength / untreated tissue strength × 100%

[0106] The results are shown in Table 1.

[0107] Table 1

[0108]

[0109]

[0110] It can be seen from the above table that the non-woven fabric bulking treatment agent prepared in Examples 1-3 of the present invention can significantly improve the hydrophilicity of the fabric, improve the whiteness, have a good hand feel, and improve the bulkiness of the fabric, have little effect on the mechanical properties of the fabric, and can also improve the mechanical properties to a certain extent.

[0111] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing a soft and fluffy treatment agent for non-woven fabrics, characterized in that: The surface of nano-silica is modified with aminosilane and then subjected to hyperbranching reaction with dimethylol propionic acid, further modified with a silane coupling agent, reacted with the reaction product of vegetable oil and diethylenetriamine, and then evenly mixed with glycerol, water, Tween-80 and amino silicone oil, and emulsified to obtain a soft and fluffy treatment agent for non-woven fabrics.

2. The preparation method according to claim 1, characterized in that: The following steps are involved: S1. Preparation of amino-modified nano-silica: adding nano-silica and aminosilane to ethanol, heating and stirring to react, centrifuging, washing, and drying to obtain amino-modified nano-silica; S2. Preparation of hyperbranched nano-silica: adding amino-modified nano-silica to toluene, adding dimethylol propionic acid and p-toluenesulfonic acid, heating under reflux with stirring, centrifuging, washing, and drying to obtain hyperbranched nano-silica; S3. Preparation of silane coupling agent modified nano-silica: adding the composite silane coupling agent to ethanol, adding hyperbranched nano-silica, heating and stirring the reaction, centrifuging, washing, and drying to obtain modified nano-silica; S4. Preparation of intermediate: Mix vegetable oil and diethylenetriamine, heat and stir to react, add modified nano-silica, stir to react at room temperature, centrifuge, wash, and dry to obtain an intermediate; S5. Preparation of a soft and fluffy treatment agent for non-woven fabrics: Glycerin, water, Tween-80, amino silicone oil and an intermediate are uniformly mixed and emulsified to prepare a soft and fluffy treatment agent for non-woven fabrics.

3. The preparation method according to claim 2, characterized in that: The mass ratio of the nano-silica to the aminosilane in step S1 is 10:2-3, the average particle size of the nano-silica is 80-150 nm, the temperature of the heating and stirring reaction is 40-50° C., and the time is 1-3 h. The aminosilane is selected from at least one of γ-aminopropyltrimethoxysilane, γ-aminopropyltriethoxysilane, N-β (aminoethyl)-γ-aminopropyltrimethoxysilane, N-β (aminoethyl)-γ-aminopropyltriethoxysilane, N-β (aminoethyl)-γ-aminopropylmethyldimethoxysilane, N-β (aminoethyl)-γ-aminopropylmethyldiethoxysilane, and diethylenetriaminopropyltrimethoxysilane.

4. The preparation method according to claim 2, characterized in that: In step S2, the mass ratio of amino-modified nano-silica, dimethylolpropionic acid and p-toluenesulfonic acid is 5-7:22-24:0.1-0.2, and the reflux heating stirring reaction time is 4-6h.

5. The preparation method according to claim 2, characterized in that: In step S3, the mass ratio of the composite silane coupling agent to the hyperbranched nano-silica is 2-3:10-12, the temperature of the heating and stirring reaction is 45-55° C., the time is 1-3 h, and the composite silane coupling agent is a mixture of KH550 and KH560, with a mass ratio of 3-5:

10.

6. The preparation method according to claim 2, characterized in that: The mass ratio of the vegetable oil, diethylenetriamine and modified nano-silica in step S4 is 10:4-7:25-30, the temperature of the heating and stirring reaction is 135-145°C, the time is 4-5h, the time of the room temperature stirring reaction is 2-4h, and the vegetable oil is selected from at least one of soybean oil, peanut oil, sesame oil, rapeseed oil, linseed oil and corn oil.

7. The preparation method according to claim 2, characterized in that: In step S5, the mass ratio of glycerol, water, Tween-80, amino silicone oil and intermediate is 20-30:10-20:2-3:3-5:10-12, and the emulsification condition is 7000-8000 r / min for 10-20 min.

8. The preparation method according to claim 2, characterized in that: The specific steps include: S1. Preparation of amino-modified nano-silica: 10 parts by weight of nano-silica and 2-3 parts by weight of aminosilane were added to ethanol, heated to 40-50°C, stirred for reaction for 1-3h, centrifuged, washed, and dried to obtain amino-modified nano-silica; S2. Preparation of hyperbranched nano-silica: 5-7 parts by weight of amino-modified nano-silica was added to toluene, 22-24 parts by weight of dimethylol propionic acid and 0.1-0.2 parts by weight of p-toluenesulfonic acid were added, the reaction was stirred under reflux for 4-6h, centrifuged, washed and dried to obtain hyperbranched nano-silica; S3. Preparation of silane coupling agent modified nano-silica: 2-3 parts by weight of the composite silane coupling agent was added to ethanol, 10-12 parts by weight of hyperbranched nano-silica was added, heated to 45-55 ° C, stirred for 1-3h, centrifuged, washed, and dried to obtain modified nano-silica; The composite silane coupling agent is a mixture of KH550 and KH560, with a mass ratio of 3-5:10; S4. Preparation of intermediate: 10 parts by weight of vegetable oil and 4-7 parts by weight of diethylenetriamine were mixed, heated to 135-145 ° C, stirred for 4-5h, added 25-30 parts by weight of modified nano-silica, stirred at room temperature for 2-4h, centrifuged, washed, and dried to obtain an intermediate; S5. Preparation of a soft and fluffy treatment agent for non-woven fabrics: 20-30 parts by weight of glycerol, 10-20 parts by weight of water, 2-3 parts by weight of Tween-80, 3-5 parts by weight of amino silicone oil and 10-12 parts by weight of the intermediate are mixed evenly, and emulsified at 7000-8000 r / min for 10-20 min to obtain a soft and fluffy treatment agent for non-woven fabrics.

9. A soft and fluffy treating agent for non-woven fabrics obtained by the preparation method according to any one of claims 1 to 8.

Citation Information

Patent Citations

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