阅读说明：本技术 一种防水防油面料的制备方法 (Preparation method of waterproof and oilproof fabric ) 是由 吴会明 朱文刚 夏忠勇 王利美 黄达河 张成胜 于 2020-10-30 设计创作，主要内容包括：本发明通过一种防水防油面料的制备方法,涉及面料生产技术领域。本申请包括以下步骤：(1)将三氟丙基甲基环三硅氧烷、八甲基环四硅氧烷、四甲基四乙烯基环四硅氧烷、偶联剂,反应后,得到含氟羧基硅油；(2)将甲基丙烯酸丁酯、丙烯酸丁酯等混合,发生聚合反应,得到含羟基丙烯酸树脂溶液；(3)将含氟羧基硅油、含羟基丙烯酸树脂溶液按照质量比为1:1的比例混合后加入乳化剂进行乳化,得到第一整理液；(4)将水性聚氨酯、二氧化钛、氧化锡锑混合配置成第二整理液；(5)将面料依次浸润于第二整理液、第一整理液中,然后进行烘干。本发明的面料具有非常好的防水防油的作用,降低布料的导热系数,提高布料的隔热性能。(The invention relates to the technical field of fabric production, in particular to a preparation method of a waterproof and oilproof fabric. The method comprises the following steps: (1) reacting trifluoropropylmethylcyclotrisiloxane, octamethylcyclotetrasiloxane, tetramethyltetravinylcyclotetrasiloxane and coupling agent to obtain fluorine-containing carboxyl silicone oil; (2) mixing butyl methacrylate, butyl acrylate and the like, and carrying out polymerization reaction to obtain a hydroxyl-containing acrylic resin solution; (3) mixing fluorine-containing carboxyl silicone oil and hydroxyl-containing acrylic resin solution according to the mass ratio of 1:1, and adding an emulsifier for emulsification to obtain a first finishing liquid; (4) mixing waterborne polyurethane, titanium dioxide and tin antimony oxide to prepare second finishing liquid; (5) and (3) soaking the fabric in the second finishing liquid and the first finishing liquid in sequence, and then drying. The fabric has good waterproof and oilproof effects, reduces the heat conductivity coefficient of the fabric, and improves the heat insulation performance of the fabric.)

1. The preparation method of the waterproof and oilproof fabric is characterized by comprising the following steps:

(1) preparing a first solution: heating and stirring trifluoropropylmethylcyclotrisiloxane, octamethylcyclotetrasiloxane, tetramethyltetravinylcyclotetrasiloxane and coupling agent, refluxing and condensing, heating, adding a first catalyst, and adding a second catalyst after 20-30min to obtain the fluorine-containing carboxyl silicone oil;

(2) preparing a second solution: uniformly mixing butyl methacrylate, butyl acrylate, methyl methacrylate, styrene and hydroxypropyl acrylate, adding an initiator, heating, and carrying out polymerization reaction to obtain a hydroxyl-containing acrylic resin solution;

(3) emulsifying the solution: mixing fluorine-containing carboxyl silicone oil and hydroxyl-containing acrylic resin solution according to the mass ratio of 1:1, and adding an emulsifier for emulsification to obtain a first finishing liquid;

(4) preparing a second finishing liquid: mixing waterborne polyurethane, titanium dioxide and tin antimony oxide to prepare second finishing liquid;

(5) soaking the fabric in the second finishing liquid for 2-3min, pressurizing to remove redundant liquid, then performing primary pre-drying and primary baking, and cooling to obtain the fabric with the heat insulation layer;

(6) and soaking the fabric with the heat-insulating layer in the first finishing liquid for 30-45s, taking out, pressurizing to remove redundant liquid, then performing secondary pre-drying and secondary baking, and cooling to obtain the waterproof and oilproof fabric with the heat-insulating layer.

2. The preparation method of the water-proof and oil-proof fabric according to claim 1, wherein the mass ratio of the water-based polyurethane to the titanium dioxide to the tin antimony oxide in the second finishing liquid is 90:5-6: 7-9.

3. The preparation method of the water-proof and oil-proof fabric according to claim 1, wherein the temperature of the first prebaking in the step (6) is 85-95 ℃ and the time is 5 min.

4. The preparation method of the water-proof and oil-proof fabric as claimed in claim 3, wherein the temperature of the first baking in the step (6) is 100-110 ℃, and the time is 3 min.

5. The preparation method of the water-proof and oil-proof fabric as claimed in claim 1, wherein the temperature of the second pre-drying in the step (5) is 110-130 ℃ for 4 min.

6. The preparation method of the water-proof and oil-proof fabric as claimed in claim 5, wherein the temperature of the second baking in the step (5) is 120-140 ℃ for 3 min.

7. The preparation method of the water-proof and oil-proof fabric according to claim 1, wherein the thickness of the heat insulation layer is 28-35 μm.

8. The method for preparing the water-proof and oil-proof fabric according to claim 1, wherein the concentration of the first finishing liquid is 2.3-2.6%.

9. The method for preparing the water-proof and oil-proof fabric according to claim 1, wherein the coupling agent is gamma-aminopropyl triethoxysilane.

10. The method for preparing the water and oil repellent fabric according to claim 9, wherein the first catalyst is tetramethylammonium hydroxide and the second catalyst is maleic anhydride.

Technical Field

The invention relates to the technical field of fabric production, in particular to a preparation method of a waterproof and oilproof fabric.

Background

The fabric is a basic material for making clothes, and different fabrics can be used for making clothes with different functions, such as waterproof clothes, warm-keeping clothes and quick-drying clothes. The common garment materials are divided into two large series; the woven fabric is mainly used for coats and shirts of clothes. Knitting the fabric: the technical development of the underwear and the sports series clothes of the clothes, however, the knitted fabric is also developed to be thick and stiff, the knitted underwear is gradually externalized, and the knitting fabric tatting method becomes the supplement of the outer clothes. With the improvement of the life quality of modern people, the wearing requirements of the modern people are also higher and higher, the modern people are not limited to the shape and style of the clothes, and whether the fabric of the clothes is comfortable or not and whether the fabric is environment-friendly or not are emphasized.

Clothing fabrics are commonly used.

First) cotton type fabric, which is a fabric woven by cotton yarn or cotton and cotton type chemical fiber blended yarn. The fabric is good in air permeability, good in moisture absorption and comfortable to wear, and is popular fabric with strong practicability. Can be divided into two categories of pure cotton products and cotton blending.

Secondly), the hemp type fabric is a pure hemp fabric woven by hemp fibers and a fabric formed by blending or interweaving hemp and other fibers, which are collectively called the hemp type fabric. The common characteristics of the hemp type fabrics are that the fabrics are hard and tough, rough and stiff, cool and comfortable, and have good moisture absorption, and the fabrics are ideal summer clothing fabrics, and the hemp type fabrics can be divided into two types of pure spinning and blended spinning.

Thirdly), the silk type fabric is a high-grade variety in textiles. Mainly refers to a fabric which takes mulberry silk, tussah silk, rayon and synthetic fiber filaments as main raw materials. It has the advantages of thinness, lightness, softness, smoothness, elegance, gorgeous and comfort.

Fourth) the wool type fabric, the fabric made of wool, rabbit hair, camel hair, hair type chemical fibre as the main raw materials, generally regard wool as the principal, it is the top-grade garment facing material of the whole year, it has elasticity good, crease-resist, stiff and smooth, wear-resisting, the warmth retention is strong, advantages such as being comfortable and esthetic, color and luster are pure, welcome by consumers.

Fifthly), the purified fiber fabric is the chemical fiber fabric which is popular with people due to the advantages of high fastness, good elasticity, stiffness, wear resistance, washing resistance and easy storage and collection. The purified fiber fabric is a fabric woven by pure chemical fibers. The properties of which are determined by the properties of the chemical fibers themselves. The chemical fiber can be processed into certain length according to different requirements, and can be woven into fabrics of silk-like, cotton-like, hemp-like, elastic wool-like, medium-length wool-like and the like according to different processes.

The functionalization of the fabric is the basis for realizing the functionalization of the clothes, and the functionalization of the clothes can be realized by improving the surface property of the fabric.

A published chinese patent application No. cn201811370749.x discloses a waterproof fabric. The invention relates to a waterproof fabric, and belongs to the technical field of textile fabrics. The waterproof fabric sequentially comprises a sweat absorbing layer, a breathable layer, a waterproof layer and a quick drying layer from inside to outside, wherein the sweat absorbing layer is 1-2mm thick, the breathable layer is 0.15-0.25mm thick, the waterproof layer is 0.05-0.12mm thick, and the quick drying layer is 0.05-0.5mm thick, wherein the waterproof layer is prepared from the following raw materials in parts by weight: 30-40 parts of terylene, 10-20 parts of vinylon, 10-20 parts of carbon fiber, 20-30 parts of sodium ortho-hydroxybenzoate, 5-10 parts of silicon dioxide, 30-50 parts of waterproof concentrated solution resin, 3-8 parts of plasticizer, 10-20 parts of water-based silicone oil and 5-10 parts of softener. The waterproof fabric is good in waterproof effect and high in comfort level. The fabric has certain waterproof capability but no oil-proof capability, and the thickness of the fabric is very thick to realize the multifunctional fabric of the fabric, so that the comfort is affected, and in addition, the heat-insulating property of the fabric is not good for the clothes with heat-insulating requirement.

In the prior art, the fabric has poor functionalization, small water contact angle on the fabric and poor water and oil resistance, and the fabric which is required to be made of the material has limited heat preservation capability.

Disclosure of Invention

In view of the above, the invention provides a preparation method of a waterproof and oilproof fabric, which has a very good waterproof and oilproof effect, and after the second finishing liquid and the first finishing liquid are coated, the fabric is equivalent to two protective layers, namely a waterproof and oilproof layer and a heat insulation layer from outside to inside, when the fabric is contacted with water or oil stains, water molecules and oil molecules cannot enter the fabric due to a large contact angle of the surface layer of the fabric, so that the fabric can effectively prevent water and oil. In addition, titanium dioxide and tin antimony oxide are added into the heat insulation layer as additives of the waterborne polyurethane, so that the heat conductivity coefficient of the cloth material is reduced, and the heat insulation performance of the cloth material is improved.

The invention relates to a preparation method of a waterproof and oilproof fabric, which comprises the following steps:

(1) preparing a first solution: mixing trifluoropropylmethyl cyclotrisiloxane, octamethylcyclotetrasiloxane, tetramethyltetravinylcyclotetrasiloxane and coupling agent, heating and stirring, wherein the coupling agent can be gamma-aminopropyltriethoxysilane KH-550, refluxing and condensing, heating to 110-;

(2) preparing a second solution: uniformly mixing butyl methacrylate, butyl acrylate, methyl methacrylate, styrene and hydroxypropyl acrylate, adding an initiator ammonium persulfate aqueous solution, heating to 81-83 ℃, and carrying out polymerization reaction to obtain a hydroxyl-containing acrylic resin solution;

(3) emulsifying the solution: mixing fluorine-containing carboxyl silicone oil and hydroxyl-containing acrylic resin solution according to a mass ratio of 1:1, and adding an emulsifier for emulsification to obtain a first finishing liquid, wherein the emulsifier can be AEO3 or AEO 9;

the first finishing liquid contains rich Si-O bonds and C-F bonds, and a large number of polymers of C-F chain links are arranged on the outermost layer of the functional coating film in a C-F form on the surface of the functional coating film, so that the interface of the fluorine-containing polymer in the dyeing and finishing process is greatly reduced, and the textile obtains good waterproof and oilproof functions.

Because the bond energy of the Si-O bond is high, the molecular chain flexibility is large, the fabric is high-temperature resistant and low in surface energy, and the fabric has good waterproofness, high-temperature resistance, stain resistance and the like by coating a layer of polymer containing the high Si-O bond on the surface of the fabric. When the first finishing liquid is coated on the surface of the fabric, the compactness of the fabric can be improved, the water absorption rate is obviously reduced, and the penetration of the liquid containing oleophylic groups is prevented. When the polymer is formed into a film on the fiber surface of the fabric, functional groups contained in molecular side chains of the polymer are arranged towards the air direction, active groups are easy to react and crosslink and are easy to bond with the fiber, and finally a smooth film is covered on the fiber surface to play a role in blocking water and oil drops.

(4) Preparing a second finishing liquid: mixing waterborne polyurethane, titanium dioxide, tin antimony oxide and a thickening agent to prepare a second finishing liquid, wherein the mass ratio of the waterborne polyurethane to the titanium dioxide to the tin antimony oxide is 90:5-6: 7-9;

the water-based polyurethane mixed with titanium dioxide and tin antimony oxide can play a good role in heat insulation and ultraviolet resistance, has a good ageing resistance and an excellent ultraviolet resistance function, and has good heat insulation performance due to the fact that the titanium dioxide and the tin antimony oxide are used as fillers.

(5) Soaking the fabric in second finishing liquid for 2-3min, wherein the second finishing liquid is not absorbed by the first finishing liquid, so that the fabric is soaked in the second finishing liquid for a long time, pressurizing to remove redundant liquid, then carrying out primary pre-drying and primary baking, wherein the temperature of the primary pre-drying is 85-95 ℃ for 5min, the temperature of the primary baking is 100-110 ℃ for 3min, and cooling to obtain the fabric with a heat insulation layer, wherein the thickness of the heat insulation layer is 28-35 mu m;

baking refers to a dyeing and finishing process that promotes the fixation of a pigment applied to a fabric or chemically reacts a finishing agent on the fabric through dry heat treatment. In the paint dyeing and printing process, baking is a process of promoting a cross-linking reaction of an adhesive and bonding, cross-linking and fixing pigment particles and fibers; in the crease-resistant finishing process of fabric, baking is the process of promoting the resin initial condensate of finishing agent to produce cross-linking reaction with fiber or the initial condensate to polymerize to produce high polymer in the presence of catalyst. The method comprises the steps of firstly carrying out a low-temperature pre-baking process to prevent resin or paint from rapidly migrating to the surface of the fabric to cause resins on the surface of a shade and a sun and the surface, and then carrying out a high-temperature baking process to achieve the purpose of promoting a crosslinking chemical reaction.

(6) Soaking the fabric with the heat-insulating layer in a first finishing liquid for 30-45s, taking out the fabric, wherein the concentration of the first finishing liquid is 2.3-2.6%, extruding and pressurizing the fabric by using a small roller press to remove redundant liquid, then carrying out secondary pre-drying and secondary baking, wherein the temperature of the secondary pre-drying is 110-.

The fabric is equivalent to two protective layers, namely a waterproof and oil-proof layer and a heat-insulating layer from outside to inside after the second finishing liquid and the first finishing liquid are coated, and when the fabric contacts water or oil stains, water molecules and oil molecules cannot enter the fabric due to the fact that the contact angle of the surface layer of the fabric is large, and the fabric can effectively prevent water and oil. In addition, titanium dioxide and antimony tin oxide are added into the heat insulation layer as additives of the waterborne polyurethane, so that the heat insulation performance of the material is improved, and the heat conductivity coefficient of the cloth is reduced mainly due to the addition of the additives.

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions of the embodiments of the present application will be clearly and completely described below, and it is obvious that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.

Example 1

A preparation method of a waterproof and oilproof fabric comprises the following steps:

(1) preparing a first solution: mixing trifluoropropylmethylcyclotrisiloxane, octamethylcyclotetrasiloxane, tetramethyltetravinylcyclotetrasiloxane and coupling agent, heating and stirring, wherein the coupling agent can be gamma-aminopropyltriethoxysilane KH-550, refluxing and condensing, heating to 110 ℃, adding a first catalyst, wherein the first catalyst can be tetramethylammonium hydroxide, heating to 130 ℃, carrying out polymerization reaction, decomposing the catalyst for 20min, cooling to about 70 ℃, and adding a second catalyst, namely maleic anhydride, to obtain the fluorine-containing carboxyl silicone oil;

(2) preparing a second solution: uniformly mixing butyl methacrylate, butyl acrylate, methyl methacrylate, styrene and hydroxypropyl acrylate, adding an initiator ammonium persulfate aqueous solution, heating to 82 ℃, and carrying out polymerization reaction to obtain a hydroxyl-containing acrylic resin solution;

(3) emulsifying the solution: mixing fluorine-containing carboxyl silicone oil and hydroxyl-containing acrylic resin solution according to a mass ratio of 1:1, and adding an emulsifier for emulsification to obtain a first finishing liquid, wherein the emulsifier can be AEO3 or AEO 9;

(4) preparing a second finishing liquid: mixing waterborne polyurethane, titanium dioxide, tin antimony oxide and a thickening agent to prepare second finishing liquor, wherein the mass ratio of the waterborne polyurethane to the titanium dioxide to the tin antimony oxide is 90:5: 7;

(5) soaking the fabric in second finishing liquid for 2min, wherein the second finishing liquid is not absorbed by the first finishing liquid, so that the fabric is soaked in the second finishing liquid for a long time, pressurizing to remove redundant liquid, then carrying out first pre-drying and first baking, wherein the temperature of the first pre-drying is 85 ℃, the time is 5min, the temperature of the first baking is 100 ℃, the time is 3min, and cooling to obtain the fabric with a heat insulation layer, wherein the thickness of the heat insulation layer is 28 microns;

(6) soaking the fabric with the heat-insulating layer in a first finishing liquid for 30s, taking out the fabric, wherein the concentration of the first finishing liquid is 2.3%, extruding and pressurizing the fabric by using a small roller press to remove redundant liquid, then carrying out secondary pre-drying and secondary baking, wherein the temperature of the secondary pre-drying is 110 ℃ for 4min, the temperature of the secondary baking is 120 ℃ for 3min, and cooling the fabric to obtain the waterproof and oilproof fabric with the heat-insulating layer.

Example 2

A preparation method of a waterproof and oilproof fabric comprises the following steps:

(1) preparing a first solution: mixing trifluoropropylmethylcyclotrisiloxane, octamethylcyclotetrasiloxane, tetramethyltetravinylcyclotetrasiloxane and coupling agent, heating and stirring, wherein the coupling agent can be gamma-aminopropyltriethoxysilane KH-550, refluxing and condensing, heating to 115 ℃, adding a first catalyst, wherein the first catalyst can be tetramethylammonium hydroxide, heating to 140 ℃, carrying out polymerization reaction, decomposing the catalyst for 30min, cooling to about 70 ℃, and adding a second catalyst, namely maleic anhydride, to obtain the fluorine-containing carboxyl silicone oil;

(2) preparing a second solution: uniformly mixing butyl methacrylate, butyl acrylate, methyl methacrylate, styrene and hydroxypropyl acrylate, adding an initiator ammonium persulfate aqueous solution, heating to 82 ℃, and carrying out polymerization reaction to obtain a hydroxyl-containing acrylic resin solution;

(3) emulsifying the solution: mixing fluorine-containing carboxyl silicone oil and hydroxyl-containing acrylic resin solution according to a mass ratio of 1:1, and adding an emulsifier for emulsification to obtain a first finishing liquid, wherein the emulsifier can be AEO3 or AEO 9;

(4) preparing a second finishing liquid: mixing waterborne polyurethane, titanium dioxide, tin antimony oxide and a thickening agent to prepare a second finishing liquid, wherein the mass ratio of the waterborne polyurethane to the titanium dioxide to the tin antimony oxide is 90: 6: 9;

(5) soaking the fabric in second finishing liquid for 3min, wherein the second finishing liquid is not absorbed by the first finishing liquid, so that the fabric is soaked in the second finishing liquid for a long time, pressurizing to remove redundant liquid, then carrying out first pre-drying and first baking, wherein the temperature of the first pre-drying is 95 ℃, the time is 5min, the temperature of the first baking is 110 ℃, the time is 3min, and cooling to obtain the fabric with a heat insulation layer, wherein the thickness of the heat insulation layer is 35 mu m;

(6) soaking the fabric with the heat-insulating layer in a first finishing liquid for 45s, taking out the fabric, wherein the concentration of the first finishing liquid is 2.6%, extruding and pressurizing the fabric by using a small roller press to remove redundant liquid, then carrying out secondary pre-drying and secondary baking, wherein the temperature of the secondary pre-drying is 130 ℃, the time is 4min, the temperature of the secondary baking is 140 ℃, the time is 3min, and cooling to obtain the waterproof and oilproof fabric with the heat-insulating layer.

Example 3

A preparation method of a waterproof and oilproof fabric comprises the following steps:

(1) preparing a first solution: mixing trifluoropropylmethylcyclotrisiloxane, octamethylcyclotetrasiloxane, tetramethyltetravinylcyclotetrasiloxane and coupling agent, heating and stirring, wherein the coupling agent can be gamma-aminopropyltriethoxysilane KH-550, refluxing and condensing, heating to 110 ℃, adding a first catalyst, the first catalyst can be tetramethylammonium hydroxide, heating to 130 ℃, carrying out polymerization reaction, decomposing the catalyst for 25min, cooling to about 70 ℃, and adding a second catalyst, namely maleic anhydride, to obtain the fluorine-containing carboxyl silicone oil;

(2) preparing a second solution: uniformly mixing butyl methacrylate, butyl acrylate, methyl methacrylate, styrene and hydroxypropyl acrylate, adding an initiator ammonium persulfate aqueous solution, heating to 83 ℃, and carrying out polymerization reaction to obtain a hydroxyl-containing acrylic resin solution;

(3) emulsifying the solution: mixing fluorine-containing carboxyl silicone oil and hydroxyl-containing acrylic resin solution according to a mass ratio of 1:1, and adding an emulsifier for emulsification to obtain a first finishing liquid, wherein the emulsifier can be AEO3 or AEO 9;

(4) preparing a second finishing liquid: mixing waterborne polyurethane, titanium dioxide, tin antimony oxide and a thickening agent to prepare a second finishing liquid, wherein the mass ratio of the waterborne polyurethane to the titanium dioxide to the tin antimony oxide is 90:5.5: 8;

(5) soaking the fabric in second finishing liquid for 2.5min, wherein the second finishing liquid is not absorbed by the first finishing liquid, so that the fabric is soaked in the second finishing liquid for a long time, pressurizing to remove redundant liquid, then carrying out primary pre-drying and primary baking, wherein the temperature of the primary pre-drying is 88 ℃ for 5min, the temperature of the primary baking is 105 ℃ for 3min, and cooling to obtain the fabric with a heat insulation layer, wherein the thickness of the heat insulation layer is 30 mu m;

(6) soaking the fabric with the heat-insulating layer in a first finishing liquid for 35s, taking out the fabric, wherein the concentration of the first finishing liquid is 2.5%, extruding and pressurizing the fabric by using a small roller press to remove redundant liquid, then carrying out secondary pre-drying and secondary baking, wherein the temperature of the secondary pre-drying is 120 ℃, the time is 4min, the temperature of the secondary baking is 130 ℃, the time is 3min, and cooling to obtain the waterproof and oilproof fabric with the heat-insulating layer.

Comparative example

The same fabric as in example 3 was finished with a commercially available water-repellent finishing agent for 2 times. The temperatures of pre-baking and baking were the same as in example 3.

And (3) taking the fabric obtained in the examples 1 to 3 and testing the waterproof and oilproof effects and the heat insulation effect of the fabric processed in the comparative example.

Referring to GB/T4744-2013 hydrostatic pressure method for detecting and evaluating the water resistance of textiles, a YG (B) 812D digital fabric water permeability tester is adopted to test the water resistance of the finished fabric.

The results of the measurements are as follows:

adopt sealed thermal-insulated case to carry out heat-proof quality test, put the cloth that will await measuring in the intermediate position of case, the cloth can be divided into two parts with the case, prevents the rising temperature device in the left side, and the right side sets up temperature probe, measures the temperature on right side after 30min and raises the temperature to 50 ℃.

The results of the measurement are as follows;

the results show that the fabric prepared by the embodiment of the invention has good water resistance and oil resistance, and good heat insulation.

The fabric is equivalent to two protective layers, namely a waterproof and oil-proof layer and a heat-insulating layer from outside to inside after the second finishing liquid and the first finishing liquid are coated, and when the fabric contacts water or oil stains, water molecules and oil molecules cannot enter the fabric due to the fact that the contact angle of the surface layer of the fabric is large, and the fabric can effectively prevent water and oil. In addition, titanium dioxide and antimony tin oxide are added into the heat insulation layer as additives of the waterborne polyurethane, so that the heat insulation performance of the material is improved, and the heat conductivity coefficient of the cloth is reduced mainly due to the addition of the additives.

The present invention is not limited to the above-described specific embodiments, and various modifications and variations are possible. Any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention should be included in the scope of the present invention.