CN110952336A - Three-proofing finishing agent for fabric, and preparation method and use method thereof - Google Patents
Three-proofing finishing agent for fabric, and preparation method and use method thereof Download PDFInfo
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- CN110952336A CN110952336A CN201811124690.6A CN201811124690A CN110952336A CN 110952336 A CN110952336 A CN 110952336A CN 201811124690 A CN201811124690 A CN 201811124690A CN 110952336 A CN110952336 A CN 110952336A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/6436—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing amino groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
- C08G77/382—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon
- C08G77/385—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon containing halogens
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
- C08G77/382—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon
- C08G77/388—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon containing nitrogen
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/01—Stain or soil resistance
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/11—Oleophobic properties
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/35—Abrasion, pilling or fibrillation resistance
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- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention provides a three-proofing finishing agent for fabric, a preparation method and a use method thereof. The finishing process of the three-proofing finishing agent provided by the invention can be realized at 0-50 ℃, and the three-proofing finishing agent has wide application fields, including the fields of automobiles, high-speed rails, clothes, home furnishings and the like. The three-proofing finishing agent provided by the invention has the advantages of simple and reasonable production process, low product cost, good three-proofing performance and high friction resistance, and does not influence the original finishing agent with the performances of fabric color, softness, air permeability, strength and the like; the used solution solvent adopts an absolute ethyl alcohol solvent, so that the pollution is avoided, no pungent smell exists, and the cost is low; and the three-proofing finishing agent does not contain toxic compounds such as APEO, PFOA, PFOS and the like, is non-toxic and harmless, has no stimulation to skin, and has the characteristics of ecological environmental protection and guarantee of health and safety of human bodies.
Description
Technical Field
The invention belongs to the technical field of fabric after-finishing, and particularly relates to a three-proofing finishing agent for fabric, and a preparation method and a use method thereof.
Background
In recent years, with the improvement of living standard, people have more and more pursued the functions of the automotive interior fabric. The investigation shows that the problems that the surface is not waterproof, residual liquid is difficult to remove, fine particles are easy to be embedded into gaps, frequent cleaning is needed, cleaning work is troublesome and the like are main pain points of users to the existing fabric. Through carrying out three proofings arrangement to the fabric surface, can realize waterproof grease proofing antifouling function, can solve user's pain point problem. The three-proofing finishing is mainly based on the lotus leaf bionic principle, a rough nano structure is constructed on the surface of fabric fibers and low surface energy substances are modified through physical or chemical methods and the like, so that a hydrophobic material is formed on the surface of the fabric, the water contact angle of the fabric is larger than 130 degrees, the water rolling angle is smaller than 15 degrees, and the three-proofing finishing has extremely strong water, oil and stain resistance functions and the like.
The prior three-proofing finishing of the fabric is generally carried out by padding treatment in the production process of the fabric and then tentering and shaping at the high temperature of 150-170 ℃, so that the three-proofing finishing of the fabric has high equipment requirement and complex process. Patent CN105484018B provides a preparation method of a stain-release jacquard fabric, which is characterized by comprising the following steps: the first step is as follows: preparing a finishing liquid: taking modified SiO2The hydrosol, the hydrophilic component and the water are mixed according to the weight ratio of 3-5: 1-3: 92-96, and stirring to obtain a finishing liquid; the modified SiO2The preparation method of the hydrosol comprises the following steps: mixing 1-4 g of precursor, 0.2-1.2 CMC anionic surfactant and 80-120 g of water, and violently stirring for 0.5-2 h at 20-50 ℃; wherein CMC is the critical micelle concentration of the surfactant; dropwise adding catalyst ammonia water, stirring for 1-6 h, adding 1-5 g of modifier long-chain alkyl siloxane, and continuously stirring for 1-5 h to obtain modified SiO2Hydrosol; the hydrophilic component consists of one of acrylic acid, methacrylic acid and hydroxyacrylic acid and one of glycerol, propylene glycol, triethanolamine and diethanolamine; the second step is that: and (3) carrying out secondary soaking and secondary rolling process finishing on the jacquard fabric by adopting the finishing liquid, and drying, wherein the rolling residue rate is 70% -80%, the drying temperature is 80 ℃, the drying time is 2-5 min, the drying temperature is 150-170 ℃, and the drying time is 1-3 min, so that the treated easy-to-clean jacquard fabric is obtained.
However, the process is complicated, in order to avoid a complicated process and simplify a use method, and a scheme of afterloading finishing is adopted by people, patent CN 107059410A provides a fabric finishing agent with waterproof, oil-proof and antifouling performances, and the fabric finishing agent comprises 1-5% of guanidine salt modified amino organic silicon, 2-5% of amino silane, 1-5% of nano silica, 20-40% of ethyl acetate, 30-40% of butyl acetate and 20-30% of ethanol in parts by mass. The preparation method comprises the following steps: mixing amino silane and nano silicon dioxide to obtain silane modified nano silicon dioxide; and mixing the silane modified nano silicon dioxide and the substances according to a ratio to obtain the fabric finishing agent with three-proofing performance. The finishing agent can be attached to the surfaces of shoes, clothes and other fabrics by direct coating, spraying, dipping and other methods, and the dried fabrics have three-proofing performance and do not need secondary finishing. Although the scheme adopts a simple process to realize three-proofing finishing of the fabric, the proportion of silane and functional monomers in the finishing agent is large, so that the cost is high; in addition, the curing time of this technique is long and the abrasion resistance is poor. Therefore, the formula and the process of the finishing agent need to be optimized, an auxiliary agent which is low in cost, long-acting and wear-resistant, can be implemented at 0-50 ℃ without special process equipment is developed, and when the three-proofing effect is weakened, the water-repellent, oil-repellent and antifouling functions of the fabric can be maintained by adopting a re-spraying method.
Disclosure of Invention
In view of the above, the technical problem to be solved by the invention is to provide a three-proofing finishing agent for fabric, a preparation method and a use method thereof, the finishing process of the three-proofing finishing agent for fabric can be realized at 0-50 ℃, and the three-proofing finishing agent has low cost, good three-proofing performance and high friction resistance, and does not affect the original properties of fabric such as color, softness, air permeability and strength.
The invention provides a three-proofing finishing agent for fabrics, which is prepared from the following raw materials in percentage by mass:
1-3 wt% of fluoro-silane compounds;
1-3 wt% of ester compound;
0.1-1 wt% of amino silane curing agent;
0.001 wt% -0.01 wt% of dibutyltin catalyst;
90-97 wt% of solvent;
the sum of the components is 100 wt%.
The preparation raw materials of the three-proofing finishing agent provided by the invention comprise 1-3 wt% of fluorosilane compounds, preferably 1.5-2.5 wt%, and more preferably 1.8-2.2 wt%. The fluorosilane compound is selected from one or more of perfluorooctyl triethoxysilane, perfluorooctyl trichlorosilane, perfluorodecyl triethoxysilane and perfluorohexyl trichlorosilane.
The preparation raw materials of the three-proofing finishing agent provided by the invention also comprise 1-3 wt% of ester compounds, preferably 1.5-2.5 wt%, and more preferably 1.8-2.2 wt%. The ester compound is selected from one or more of methyl methacrylate, butyl acrylate, hydroxyethyl acrylate and dodecafluoroheptyl methacrylate.
The preparation raw materials of the three-proofing finishing agent provided by the invention also comprise 0.1-1 wt% of amino silane curing agent, preferably 0.3-0.8 wt%, more preferably 0.4-0.7 wt%, wherein the amino silane curing agent is selected from one or more of aminopropyl triethoxysilane, bisamino silane coupling agent and polyamino silane coupling agent.
The preparation raw material of the three-proofing finishing agent provided by the invention also comprises 0.001-0.01 wt% of dibutyltin catalyst, preferably 0.002-0.008 wt%, more preferably 0.004-0.006 wt%, wherein the dibutyltin catalyst is selected from one or more of dibutyltin oxide, dibutyltin dichloride and dibutyltin diacetate.
The preparation raw materials of the three-proofing finishing agent provided by the invention also comprise 90-97 wt% of solvent, preferably 92-95 wt%, more preferably 93-94 wt%, wherein the solvent is selected from absolute ethyl alcohol.
The invention also provides a preparation method of the three-proofing finishing agent for the fabric, which comprises the following steps:
and mixing a fluorosilane compound, an ester compound, an amino silane curing agent, a dibutyltin catalyst and a solvent to obtain the three-proofing finishing agent for the fabric.
The invention also provides a preparation method of the three-proofing finishing agent for the fabric, which comprises the following steps:
mixing and stirring a fluorosilane compound and an ester compound for 1-3 min at normal temperature, then adding a solvent, and continuously mixing and stirring for 1-3 min at normal temperature to obtain a mixed solution;
the solvent can be completely mixed with the fluorosilane compound and the ester compound, or part of the solvent is firstly selected to be mixed with the fluorosilane compound and the ester compound, the mixture is sealed and kept stand for more than 8 hours, and then the rest solvent is added to continue mixing and stirring at normal temperature for 1-3 min to obtain a mixed solution;
adding an amino silane curing agent and a dibutyltin catalyst into the mixed solution, and mixing and stirring at normal temperature for 1-3 min to obtain a three-proofing fabric finishing agent;
the normal temperature is 25 +/-5 ℃.
The invention also provides a preparation method of the three-proofing finishing agent for the fabric, which comprises the following steps:
mixing a solvent, part of the aminosilane curing agent and part of the dibutyltin catalyst at normal temperature, standing for more than 8 hours, adding a fluorosilane compound and an ester compound, the rest of the aminosilane curing agent and the rest of the dibutyltin catalyst, and mixing and stirring at normal temperature to obtain a three-proofing fabric finishing agent; the normal temperature is 25 +/-5 ℃.
Wherein the mass ratio of the part of the amino silane curing agent to the rest of the amino silane curing agent is (30-50%): (70-50%);
the mass ratio of the part of dibutyltin catalyst to the rest dibutyltin catalyst is (30-50%): (70-50%);
the invention also provides a use method of the normal-temperature fabric three-proofing finishing agent, which comprises the following steps:
A) cleaning the surface of the fabric to enable the surface of the fabric to reach a clean state;
B) uniformly spraying the three-proofing finishing agent on the surface of the cleaned fabric;
C) the surface of the cleaned fabric sprayed with the three-proofing finishing agent is cured for 2-5 hours at 0-50 ℃.
The curing temperature is preferably 20-40 ℃, and more preferably 25-35 ℃. The curing time is preferably 3 to 4 hours.
The fabric is selected from one or more of cotton fabric, wool fabric, silk fabric and polyester fabric.
The invention provides a fabric afterfinish (namely a normal-temperature fabric three-proofing finish) and a preparation method and a use method thereof. The finishing process of the three-proofing finishing agent provided by the invention can be realized at 0-50 ℃, and the three-proofing finishing agent has wide application fields, including the fields of automobiles, high-speed rails, clothes, home furnishings and the like. The three-proofing finishing agent provided by the invention has the advantages of simple and reasonable production process, low product cost, good three-proofing performance and high friction resistance, and does not influence the original finishing agent with the performances of fabric color, softness, air permeability, strength and the like; the used solution solvent adopts an absolute ethyl alcohol solvent, so that the pollution is avoided, no pungent smell exists, and the cost is low; and the three-proofing finishing agent does not contain toxic compounds such as APEO (alkylphenol ethoxylates), PFOA (perfluorooctanoic acid and salt thereof), PFOS (perfluorooctane sulfonyl compound) and the like, is non-toxic and harmless, has no stimulation to skin, and has the characteristics of ecological environmental protection and guarantee of human health and safety.
The three-proofing finishing agent provided by the invention can be applied to the surfaces of textile interior trims such as automobile seats, ceilings, side decorative plates and the like, and can also be applied to the surfaces of materials such as Alcantara fabrics and leather. Has excellent three-proofing performance: water-proof (purified water, rain water, etc.), oil-proof (edible oil, gasoline), anti-fouling (tea beverage, soy sauce, dust particles, etc.), and easy cleaning. Simple process, low cost and suitability for large-scale production.
The results show that the three-proofing finishing agent provided by the invention has good performance after being subjected to water repellency and anti-fouling tests, ethanol resistance tests, oil repellency tests, water staining tests, wear resistance tests, contact angle tests and rolling angle tests.
1) Water repellency and stain resistance test
Cutting the finished polyester fabric raw material into samples of 100mm x 100mm, respectively dripping 3-5 ml of pollution agents (water, cola, soy sauce and hot coffee) on the surfaces of the samples, keeping the samples for 1min, then wiping the samples off by using a paper towel, and observing that almost no infiltration or stain marks are left.
2) Contact angle, roll angle test
The water contact angle of the finished polyester fabric can reach 141.5 degrees through testing, and the rolling angle can reach 15 degrees.
3) Alcohol resistance, oil repellency, Water repellency test
The ethanol resistance grade is 8 grade (GB/T24120), the oil repellency grade is 5 grade (GB/T19977) and the water pick-up grade is 4 grade (GBT4745) according to the national standard method.
4) Abrasion resistance test
According to ISO 12947-1 standard, Martindale abrasion resistance test is carried out, 12KPa is selected as pressure, and after 2 ten thousand times of circulating friction, the ethanol resistance grade is tested to be more than or equal to 2 grade (GB/T24120).
Detailed Description
For further understanding of the present invention, the three-proofing finishing agent for fabric, its preparation method and its application method are described below with reference to the following examples, and the protection scope of the present invention is not limited by the following examples.
Example 1
1. Weighing 6.3g of perfluorooctyl triethoxysilane and 3.2g of methyl methacrylate, adding into a plastic bottle, and stirring for 1min to uniformly mix;
2. weighing 190g of absolute ethyl alcohol, adding the absolute ethyl alcohol into a plastic bottle, and stirring for 1min to uniformly mix the absolute ethyl alcohol and the plastic bottle;
3. weighing 1g of aminopropyltriethoxysilane curing agent, adding into a plastic bottle, and stirring for 1min to uniformly mix;
4. dropwise adding 2 drops (about 0.05g) of dibutyltin diacetate catalyst into a plastic bottle, stirring for 1min to uniformly mix the dibutyltin diacetate catalyst and the plastic bottle to obtain a post-finishing agent, wherein the preparation process is carried out at the temperature of 25 +/-5 ℃;
5. weighing 20g of finishing agent, adding into a spray pot, uniformly spraying the finishing agent on the surface of a cotton fabric with the size of A4 paper (210mm multiplied by 297mm) under the pressure of 4-8 kg by adopting a spray head with the aperture of 1-2 mm, and curing for 2 hours at 23 ℃ to realize the three-proofing effects of 9 grades of ethanol resistance and 5 grades of oil resistance.
Example 2
1. 2.4g of perfluorooctyl triethoxysilane and 2.4g of methyl methacrylate are weighed into a plastic bottle and stirred for 1min to be uniformly mixed;
2. weighing 190g of absolute ethyl alcohol, adding the absolute ethyl alcohol into a plastic bottle, and stirring for 1min to uniformly mix the absolute ethyl alcohol and the plastic bottle;
3. weighing 0.5g of aminopropyltriethoxysilane curing agent, adding into a plastic bottle, and stirring for 1min to uniformly mix;
4. dripping 1 drop (about 0.025g) of dibutyltin diacetate catalyst into a plastic bottle, stirring for 1min to uniformly mix the dibutyltin diacetate catalyst and the plastic bottle to obtain a post-finishing agent, wherein the preparation process is carried out at the temperature of 25 +/-5 ℃;
5. weighing 20g of finishing agent, adding into a spray pot, uniformly spraying the finishing agent on the surface of a polyester fabric with the paper size of A4 (210mm multiplied by 297mm) under the pressure of 4-8 kg by adopting a spray head with the aperture of 1-2 mm, and curing for 4 hours at 10 ℃ to realize the three-proofing effects of 8-grade ethanol resistance and 4-grade oil resistance.
Example 3
1. Weighing 190g of absolute ethyl alcohol, adding into a plastic bottle, weighing 0.5g of bisaminosilane coupling agent gamma-aminopropylmethyldimethoxysilane, adding into the plastic bottle, dropwise adding 2 drops (about 0.05g) of dibutyltin oxide catalyst into the plastic bottle, stirring for 1min to uniformly mix, and sealing and placing for 8 hours at room temperature;
2. 3.2g of perfluorooctyl trichlorosilane and 3.2g of hydroxyethyl acrylate are weighed and added into a plastic bottle, and are stirred for 1min to be uniformly mixed;
3. weighing 0.5g of gamma-aminopropylmethyldimethoxysilane, adding into a plastic bottle, stirring for 1min to uniformly mix, and finishing the preparation of the afterloading finishing agent, wherein the preparation process is carried out at the temperature of 25 +/-5 ℃;
4. weighing 20g of finishing agent, adding into a spray pot, uniformly spraying the finishing agent on the surface of a polyester fabric with the paper size of A4 (210mm multiplied by 297mm) under the pressure of 4-8 kg by adopting a spray head with the aperture of 1-2 mm, and curing for 2 hours at 23 ℃ to realize the three-proofing effects of 8-grade ethanol resistance and 5-grade oil resistance.
Example 4
1. 2.4g of perfluorodecyl triethoxysilane and 2.4g of hydroxyethyl acrylate are weighed into a plastic bottle and stirred for 1min to be uniformly mixed;
2. weighing 190g of absolute ethyl alcohol, adding the absolute ethyl alcohol into a plastic bottle, heating and stirring at 50 ℃ for 30min to uniformly mix the absolute ethyl alcohol and the plastic bottle;
3. weighing 0.5g of gamma-aminopropylmethyldimethoxysilane into a plastic bottle, and stirring for 1min to uniformly mix;
4. dripping 1 drop (about 0.025g) of dibutyltin oxide catalyst into a plastic bottle, stirring for 1min to uniformly mix, and thus completing the preparation of the afterloading finishing agent, wherein the preparation process is carried out at the temperature of 25 +/-5 ℃;
5. weighing 20g of finishing agent, adding into a spray pot, uniformly spraying the finishing agent on the surface of a cotton fabric with the size of A4 paper (210mm multiplied by 297mm) under the pressure of 4-8 kg by adopting a spray head with the aperture of 1-2 mm, and curing for 5 hours at the temperature of 0 ℃ to realize the three-proofing effect of 8-grade ethanol resistance and 4-grade oil resistance.
Example 5
1. Weighing 6.4g of perfluorohexyltrichlorosilane and 3.2g of dodecafluoroheptyl methacrylate, adding into a plastic bottle, and stirring for 1min to uniformly mix;
2. weighing 10g of absolute ethyl alcohol, adding the absolute ethyl alcohol into a plastic bottle, stirring for 1min to uniformly mix the absolute ethyl alcohol and the plastic bottle, and sealing and placing the mixture for 8 hours at room temperature;
3. weighing 180g of absolute ethyl alcohol, adding the absolute ethyl alcohol into a plastic bottle, and stirring for 1min to uniformly mix the absolute ethyl alcohol and the plastic bottle;
4. weighing 1g of aminopropyltriethoxysilane curing agent, adding into a plastic bottle, and stirring for 1min to uniformly mix;
5. dripping 2 drops (about 0.05g) of dibutyltin dichloride catalyst into a plastic bottle, stirring for 1min to uniformly mix the dibutyltin dichloride catalyst and the plastic bottle to obtain a post-loading finishing agent, wherein the preparation process is carried out at the temperature of 25 +/-5 ℃;
6. weighing 20g of finishing agent, adding into a spray pot, uniformly spraying the finishing agent on the surface of a cotton fabric with the size of A4 paper (210mm multiplied by 297mm) under the pressure of 4-8 kg by adopting a spray head with the aperture of 1-2 mm, and curing for 2 hours at 50 ℃ to realize the three-prevention effect of 8-grade ethanol resistance and 4-grade oil resistance.
Example 6
1. Weighing 3.2g of perfluorohexyltrichlorosilane, 3.2g of dodecafluoroheptyl methacrylate, 1g of aminopropyltriethoxysilane curing agent, 2 drops of dibutyltin dichloride catalyst and about 0.05g of dibutyltin dichloride, and stirring for 1min to uniformly mix the components in a plastic bottle;
2. weighing 190g of absolute ethyl alcohol, stirring and dropwise adding the absolute ethyl alcohol into a plastic bottle to uniformly mix the absolute ethyl alcohol and the plastic bottle, wherein the dropwise adding of the ethyl alcohol is completed within about 2 hours, and the preparation process is carried out at the temperature of 25 +/-5 ℃;
3. weighing 20g of finishing agent, adding into a spray pot, uniformly spraying the finishing agent on the surface of a fabric with the size of A4 paper (210mm multiplied by 297mm) under the pressure of 4-8 kg by adopting a spray head with the aperture of 1-2 mm, and curing for 2h at 23 ℃ to realize the three-proofing effects of 9 grades of ethanol resistance and 5 grades of oil resistance.
Example 7
The three-proofing finishing agent prepared in the above embodiments 1 to 6 is subjected to a performance test, and the specific method is as follows:
1) water repellency and stain resistance test
Cutting the finished polyester fabric raw material into samples of 100mm x 100mm, respectively dripping 3-5 ml of pollution agents (water, cola, soy sauce and hot coffee) on the surfaces of the samples, keeping the samples for 1min, then wiping the samples off by using a paper towel, and observing that almost no infiltration or stain marks are left.
2) Contact angle, roll angle test
The water contact angle of the finished polyester fabric can reach 141.5 degrees through testing, and the rolling angle can reach 15 degrees.
3) Alcohol resistance, oil repellency, Water repellency test
According to the national standard method, an ethanol resistance grade test method GB/T24120, an oil repellency grade test method GB/T19977 and a water staining grade test method GBT4745 are respectively tested.
4) Abrasion resistance test
And performing a Martindale abrasion resistance test according to ISO 12947-1 standard, selecting 12KPa for pressure, and testing the ethanol resistance grade according to GB/T24120 after 2 ten thousand times of circulating friction.
The results are shown in Table 1
TABLE 1 Performance test results for three-proofing finishing agents of examples 1-6
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The three-proofing finishing agent for the fabric is characterized by being prepared from the following raw materials in percentage by mass:
1-3 wt% of fluoro-silane compounds;
1-3 wt% of ester compound;
0.1-1 wt% of amino silane curing agent;
0.001 wt% -0.01 wt% of dibutyltin catalyst;
90-97 wt% of solvent;
the sum of the components is 100 wt%.
2. The three-proofing finish of claim 1, wherein said fluorosilane compound is selected from one or more of perfluorooctyltriethoxysilane, perfluorooctyltrichlorosilane, perfluorodecyltriethoxysilane, and perfluorohexyltrichlorosilane.
3. The three-proofing finishing agent according to claim 1, wherein the ester compound is selected from one or more of methyl methacrylate, butyl acrylate, hydroxyethyl acrylate and dodecafluoroheptyl methacrylate.
4. The three-proofing finishing agent according to claim 1, wherein the amino silane curing agent is selected from one or more of aminopropyltriethoxysilane, bisaminosilane coupling agents and polyaminosilane coupling agents.
5. The three-proofing finish according to claim 1, wherein said dibutyltin catalyst is selected from one or more of dibutyltin oxide, dibutyltin dichloride and dibutyltin diacetate.
6. The three-proofing finish according to claim 1, wherein said solvent is selected from absolute ethyl alcohol.
7. A preparation method of the three-proofing fabric finishing agent according to any one of claims 1 to 6, characterized by comprising the following steps:
mixing and stirring a fluorosilane compound and an ester compound for 1-3 min at normal temperature, then adding a solvent, and continuously mixing and stirring for 1-3 min at normal temperature to obtain a mixed solution;
adding an amino silane curing agent and a dibutyltin catalyst into the mixed solution, and mixing and stirring at normal temperature for 1-3 min to obtain a three-proofing fabric finishing agent;
the normal temperature is 25 +/-5 ℃.
8. A preparation method of the three-proofing fabric finishing agent according to any one of claims 1 to 6, characterized by comprising the following steps:
mixing a solvent, part of the aminosilane curing agent and all or part of the dibutyltin catalyst at normal temperature, standing for more than 8 hours, adding a fluorosilane compound and an ester compound, and adding the rest of the aminosilane curing agent and the rest of the dibutyltin catalyst, mixing and stirring at normal temperature to obtain a normal-temperature fabric three-proofing finishing agent; the normal temperature is 25 +/-5 ℃.
9. A method for using the three-proofing finishing agent for the fabric according to any one of claims 1 to 6, which is characterized by comprising the following steps:
A) cleaning the surface of the fabric to enable the surface of the fabric to reach a clean state;
B) uniformly spraying the three-proofing finishing agent on the surface of the cleaned fabric;
C) the surface of the cleaned fabric sprayed with the three-proofing finishing agent is cured for 2-5 hours at 0-50 ℃.
10. The use method according to claim 9, wherein the fabric is selected from one or more of cotton fabric, wool fabric, silk fabric and polyester fabric.
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