CN114645458A - High-stain-resistance waterproof fabric and preparation process thereof - Google Patents
High-stain-resistance waterproof fabric and preparation process thereof Download PDFInfo
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- CN114645458A CN114645458A CN202111586285.8A CN202111586285A CN114645458A CN 114645458 A CN114645458 A CN 114645458A CN 202111586285 A CN202111586285 A CN 202111586285A CN 114645458 A CN114645458 A CN 114645458A
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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
- D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
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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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/58—Epoxy resins
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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
- D06M15/55—Epoxy resins
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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
- D06M2200/12—Hydrophobic properties
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Epoxy Resins (AREA)
Abstract
The invention discloses a high stain-resistant waterproof fabric and a preparation process thereof, wherein the fabric is prepared by soaking a fabric substrate in modified resin and then curing; contain the fluorine alkane structure in this modified epoxy's the molecule main chain and make modified epoxy have certain hydrophobic effect, form polysulfone structure epoxy simultaneously on the molecular chain, make further promotion of epoxy's toughness, guaranteed that the high resistant waterproof surface fabric toughness who prepares promotes, and the side chain contains a large amount of long chain alkyl, long chain alkyl has fine hydrophobic effect, make modified epoxy's hydrophobic effect further, carry out the in-process at the processing surface fabric substrate, substrate surface fabric surface adsorption modified resin, reuse diethylenetriamine solidification, make substrate surface fabric surface form hydrophobic membrane, and then reach waterproof effect, the difficult attached stain of surface fabric has been guaranteed simultaneously.
Description
Technical Field
The invention relates to the technical field of fabric preparation, in particular to a high-stain-resistance waterproof fabric and a preparation process thereof.
Background
The super-hydrophobic material has unique surface properties such as excellent waterproofness, self-cleaning and anti-fouling, and has wide application prospects in the fields of textile materials, biomedicine and the like, the super-hydrophobic property of the material surface is determined by the surface roughness and the surface free energy, the micro-nano composite structure constructed on the fabric surface is relatively complex and is not easy to realize industrial production, and the fabric style is easily influenced by the surface roughening, so that many hydrophobic materials have low free energy on the surface, and the fluorine-containing hydrophobic agent is used as a common low-surface-energy hydrophobic agent, has excellent physicochemical characteristics and is used for the construction of the hydrophobic surface of the textile, wherein the fluorine-containing acrylate polymer is one of the widely used hydrophobic agents, has excellent hydrophobicity, good adhesive capacity and film forming property, and is widely applied to the fields of coatings, leather, textiles and the like;
the existing hydrophobic fabric obtains a waterproof effect by coating a hydrophobic coating on the surface, but after the fabric is folded for multiple times, the hydrophobic coating at the folded part of the fabric is damaged, so that the hydrophobic effect is greatly reduced, and the use effect of a hydrophobic surface is further influenced;
therefore, a high stain-resistant waterproof fabric and a preparation process thereof are provided to solve the technical defects.
Disclosure of Invention
The invention aims to provide a high stain-resistant waterproof fabric and a preparation process thereof.
The purpose of the invention can be realized by the following technical scheme:
a highly stain-resistant waterproof fabric is prepared by soaking a fabric substrate in modified resin and then curing;
the high stain-resistant waterproof fabric is prepared by the following steps:
step S1: soaking the fabric base material in modified resin, and carrying out ultrasonic treatment for 3-5h at the temperature of 70-80 ℃ and the frequency of 50-60 kHz;
step S2: adding diethylenetriamine into the epoxy resin, and carrying out ultrasonic treatment for 30-40min under the condition that the frequency is 70-80 kHz;
step S3: taking out the fabric base material, vertically hanging until no liquid drips, and drying at the temperature of 30-50 ℃ to obtain the high stain-resistant waterproof fabric.
Further, the modified resin is prepared by the following steps:
step A1: uniformly mixing bisphenol AF, dichlorodiphenyl sulfone, N-methylpyrrolidone, anhydrous potassium carbonate and toluene, reacting for 2-3h under the conditions that the rotation speed is 200-plus-300 r/min and the temperature is 140-plus-150 ℃, heating to the temperature of 160-plus-170 ℃, reacting for 3-4h, heating to the temperature of 180-plus-190 ℃, reacting for 3-4h to obtain an intermediate 1, uniformly mixing the intermediate 1, hydroquinone, anhydrous potassium carbonate and toluene, reacting for 2-3h under the conditions that the rotation speed is 200-plus-300 r/min and the temperature is 140-plus-150 ℃, heating to the temperature of 160-plus-170 ℃, reacting for 3-4h, heating to the temperature of 180-plus-190 ℃, and reacting for 3-4h to obtain an intermediate 2;
the reaction process is as follows:
step A2: uniformly mixing the intermediate 2, epichlorohydrin and benzyltriethylammonium chloride, reacting for 2-4h at the rotation speed of 200-90 ℃ for 300r/min, adding a sodium hydroxide solution, continuing to react for 1-1.5h to obtain epoxy resin, adding aluminum trichloride and carbon tetrachloride into a reaction kettle, stirring and adding nitrobenzene under the condition of changing to 150-15 ℃ for 200r/min, reacting for 1-1.5h at the temperature of 40-45 ℃, filtering to remove filter residue, distilling and dissolving filtrate, mixing a substrate and deionized water, and refluxing for 10-15min at the temperature of 110-120 ℃ to obtain an intermediate 3;
the reaction process is as follows:
step A3: uniformly mixing tin powder, the intermediate 3 and concentrated hydrochloric acid, reacting for 30-40min at the conditions of the rotation speed of 150-200r/min and the temperature of 90-100 ℃, adjusting the pH value of a reaction solution to 10-11 to prepare an intermediate 4, uniformly mixing the intermediate 4, triethylamine and toluene, stirring and introducing triphosgene at the rotation speed of 200-300r/min and the temperature of 40-50 ℃ to react for 3-5h to prepare an intermediate 5, uniformly mixing the intermediate 5, deionized water, ethanol and sodium borohydride, reacting for 30-40min at the rotation speed of 200-300r/min and the temperature of 20-25 ℃, and adding a hydrochloric acid solution to uniformly mix to prepare an intermediate 6;
the reaction process is as follows:
step A4: uniformly mixing the intermediate 6, bromooctadecane, sodium hydroxide and N, N-dimethylformamide, reacting for 6-8h at the rotation speed of 150-200r/min and the temperature of 60-70 ℃ to obtain an intermediate 7, uniformly mixing the intermediate 7 and epoxy resin, introducing nitrogen for protection, reacting for 1-1.5h at the temperature of 110-120 ℃, adding dibutyltin dilaurate, and continuing to react for 1-1.5h to obtain the modified resin.
The reaction process is as follows:
further, the molar ratio of the bisphenol AF and the dichlorodiphenyl sulfone in the step A1 is 0.98:1, and the molar ratio of the intermediate 1 and the hydroquinone is 1:2.
Further, the intermediate 2, the epichlorohydrin, the benzyltriethylammonium chloride and the sodium hydroxide solution in the step A2 are used in a dosage ratio of 0.01mol:0.02mol:10.2mg:50mL, the sodium hydroxide solution is 25% by mass, the molar ratio of the aluminum trichloride to the carbon tetrachloride is 2:1, and the dosage ratio of the substrate to the deionized water is 1g:5 mL.
Further, the using amount ratio of the tin powder, the intermediate 3 and the concentrated hydrochloric acid in the step A3 is 9g:0.01mol:20mL, the mass fraction of the concentrated hydrochloric acid is 36%, the using amount molar ratio of the intermediate 4 and the triphosgene is 1:2.1, the using amount ratio of the intermediate 5, the deionized water, the ethanol, the sodium borohydride and the hydrochloric acid solution is 0.05mol:5mL:20mL:0.5g:2mL, and the mass fraction of the hydrochloric acid solution is 5%.
Further, the intermediate 6, bromooctadecane and sodium hydroxide in the step A4 are used in a molar ratio of 1:1:1, and the intermediate 7, the epoxy resin and dibutyl tin dilaurate are used in a ratio of 0.03mol:0.01mol:0.2 mL.
The invention has the following beneficial effects:
the invention provides a high stain-resistant waterproof fabric which is prepared by soaking a fabric substrate in modified resin and then curing, wherein the modified resin is prepared by taking bisphenol AF and dichlorodiphenyl sulfone as raw materials to react to prepare an intermediate 1, reacting the intermediate 1 with hydroquinone to prepare an intermediate 2, reacting the intermediate 2 with epoxy chloropropane to prepare epoxy resin, reacting carbon tetrachloride with nitrobenzene, then refluxing with deionized water to prepare an intermediate 3, reducing the intermediate 3 with tin powder to convert nitro groups on the intermediate 3 into amino groups to prepare an intermediate 4, reacting the intermediate 4 with triphosgene to convert amino groups on the intermediate 4 into isocyanate groups to prepare an intermediate 5, reacting the intermediate 5 with sodium borohydride to convert ketone groups in the intermediate 5 into alcoholic hydroxyl groups to prepare an intermediate 6, and reacting the intermediate 6 with bromooctadecane, reacting bromine atom sites on bromooctadecane with alcoholic hydroxyl groups on the intermediate 6 to prepare an intermediate 7, reacting the intermediate 7 with epoxy resin to react alcoholic hydroxyl groups on side chains of the epoxy resin with isocyanate groups on the intermediate 7 to crosslink the epoxy resin to prepare modified epoxy resin, wherein a molecular main chain of the modified epoxy resin contains a fluorine alkane structure to ensure that the modified epoxy resin has a certain hydrophobic effect, and meanwhile, a molecular chain of the modified epoxy resin forms polysulfone-structured epoxy resin to further improve the toughness of the epoxy resin and ensure that the toughness of the prepared high-stain-resistant waterproof fabric is improved, and the side chains contain a large amount of long-chain alkyl groups which have good hydrophobic effect, so that the hydrophobic effect of the modified resin is further improved, in the process of treating the fabric substrate, the surface of the substrate fabric adsorbs the modified resin, and is cured by diethylenetriamine, the hydrophobic film is formed on the surface of the base material fabric, so that the waterproof effect is achieved, and meanwhile, the fabric is not easy to adhere to stains.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and 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 invention.
Example 1
A highly stain-resistant waterproof fabric is prepared by soaking a fabric substrate in modified resin and then curing;
the high stain-resistant waterproof fabric is prepared by the following steps:
step S1: soaking the fabric base material in modified resin, and carrying out ultrasonic treatment for 3h under the conditions that the temperature is 70 ℃ and the frequency is 50 kHz;
step S2: adding diethylenetriamine into the epoxy resin, and carrying out ultrasonic treatment for 30min under the condition that the frequency is 70 kHz;
step S3: taking out the fabric base material, vertically hanging until no liquid drips, and drying at the temperature of 30 ℃ to prepare the high-stain-resistant waterproof fabric.
The modified resin is prepared by the following steps:
step A1: uniformly mixing bisphenol AF, dichlorodiphenyl sulfone, N-methylpyrrolidone, anhydrous potassium carbonate and toluene, reacting for 2 hours at the rotation speed of 200r/min and the temperature of 140 ℃, heating to the temperature of 160 ℃, reacting for 3 hours, heating to the temperature of 180 ℃, reacting for 3 hours to obtain an intermediate 1, uniformly mixing the intermediate 1, hydroquinone, anhydrous potassium carbonate and toluene, reacting for 2 hours at the rotation speed of 200r/min and the temperature of 140 ℃, heating to the temperature of 160 ℃, reacting for 3 hours, heating to the temperature of 180 ℃, and reacting for 3 hours to obtain an intermediate 2;
step A2: uniformly mixing the intermediate 2, epichlorohydrin and benzyltriethylammonium chloride, reacting for 2 hours at the rotation speed of 200r/min and the temperature of 80 ℃, adding a sodium hydroxide solution, continuing to react for 1 hour to obtain epoxy resin, adding aluminum trichloride and carbon tetrachloride into a reaction kettle, stirring and adding nitrobenzene under the conditions of conversion to 150r/min and the temperature of 10 ℃, reacting for 1 hour at the temperature of 40 ℃, filtering to remove filter residues, distilling and dissolving filtrate, mixing a substrate and deionized water, and refluxing for 10 minutes at the temperature of 110 ℃ to obtain an intermediate 3;
step A3: uniformly mixing tin powder, an intermediate 3 and concentrated hydrochloric acid, reacting for 30min at the rotation speed of 150r/min and the temperature of 90 ℃, adjusting the pH value of a reaction solution to 10 to obtain an intermediate 4, uniformly mixing the intermediate 4, triethylamine and toluene, stirring and introducing triphosgene at the rotation speed of 200r/min and the temperature of 40 ℃ to react for 3h to obtain an intermediate 5, uniformly mixing the intermediate 5, deionized water, ethanol and sodium borohydride, reacting for 30min at the rotation speed of 200r/min and the temperature of 20 ℃, adding a hydrochloric acid solution, and uniformly mixing to obtain an intermediate 6;
step A4: uniformly mixing the intermediate 6, bromooctadecane, sodium hydroxide and N, N-dimethylformamide, reacting for 6 hours at the rotation speed of 150r/min and the temperature of 60 ℃ to obtain an intermediate 7, uniformly mixing the intermediate 7 and epoxy resin, introducing nitrogen for protection, reacting for 1 hour at the temperature of 110 ℃, adding dibutyl tin dilaurate, and continuing to react for 1 hour to obtain the modified resin.
Example 2
A highly stain-resistant waterproof fabric is prepared by soaking a fabric substrate in modified resin and then curing;
the high stain-resistant waterproof fabric is prepared by the following steps:
step S1: soaking the fabric base material in modified resin, and carrying out ultrasonic treatment for 4 hours at the temperature of 75 ℃ and the frequency of 55 kHz;
step S2: adding diethylenetriamine into the epoxy resin, and carrying out ultrasonic treatment for 35min under the condition that the frequency is 75 kHz;
step S3: taking out the fabric base material, vertically hanging until no liquid drips, and drying at the temperature of 40 ℃ to obtain the high stain-resistant waterproof fabric.
The modified resin is prepared by the following steps:
step A1: uniformly mixing bisphenol AF, dichlorodiphenyl sulfone, N-methylpyrrolidone, anhydrous potassium carbonate and toluene, reacting for 2.5 hours at the rotation speed of 300r/min and the temperature of 145 ℃, heating to 165 ℃, reacting for 3.5 hours at the temperature of 185 ℃, reacting for 3.5 hours to obtain an intermediate 1, uniformly mixing the intermediate 1, hydroquinone, anhydrous potassium carbonate and toluene, reacting for 2.5 hours at the rotation speed of 200r/min and the temperature of 145 ℃, heating to 165 ℃, reacting for 3.5 hours at the temperature of 185 ℃, heating to 185 ℃, reacting for 3.5 hours to obtain an intermediate 2;
step A2: uniformly mixing the intermediate 2, epichlorohydrin and benzyltriethylammonium chloride, reacting for 3 hours at the rotation speed of 300r/min and the temperature of 85 ℃, adding a sodium hydroxide solution, continuing to react for 1.3 hours to obtain epoxy resin, adding aluminum trichloride and carbon tetrachloride into a reaction kettle, stirring and adding nitrobenzene under the conditions of changing to 180r/min and the temperature of 13 ℃, reacting for 1.3 hours at the temperature of 43 ℃, filtering to remove filter residues, distilling and dissolving filtrate, mixing a substrate with deionized water, and refluxing for 13 minutes at the temperature of 115 ℃ to obtain an intermediate 3;
step A3: uniformly mixing tin powder, the intermediate 3 and concentrated hydrochloric acid, reacting for 35min at the rotation speed of 180r/min and the temperature of 95 ℃, adjusting the pH value of a reaction solution to be 11 to obtain an intermediate 4, uniformly mixing the intermediate 4, triethylamine and toluene, stirring and introducing triphosgene at the rotation speed of 300r/min and the temperature of 45 ℃ to react for 4h to obtain an intermediate 5, uniformly mixing the intermediate 5, deionized water, ethanol and sodium borohydride, reacting for 35min at the rotation speed of 300r/min and the temperature of 23 ℃, adding a hydrochloric acid solution, and uniformly mixing to obtain an intermediate 6;
step A4: uniformly mixing the intermediate 6, bromooctadecane, sodium hydroxide and N, N-dimethylformamide, reacting for 7 hours at the rotation speed of 180r/min and the temperature of 65 ℃ to obtain an intermediate 7, uniformly mixing the intermediate 7 and epoxy resin, introducing nitrogen for protection, reacting for 1.3 hours at the temperature of 115 ℃, adding dibutyltin dilaurate, and continuously reacting for 1.3 hours to obtain the modified resin.
Example 3
A high stain-resistant waterproof fabric is prepared by soaking a fabric base material in modified resin and then curing;
the high stain-resistant waterproof fabric is prepared by the following steps:
step S1: soaking the fabric base material in modified resin, and carrying out ultrasonic treatment for 5 hours at the temperature of 80 ℃ and the frequency of 60 kHz;
step S2: adding diethylenetriamine into the epoxy resin, and carrying out ultrasonic treatment for 40min under the condition that the frequency is 80 kHz;
step S3: taking out the fabric base material, vertically hanging until no liquid drips, and drying at the temperature of 50 ℃ to obtain the high stain-resistant waterproof fabric.
The modified resin is prepared by the following steps:
step A1: uniformly mixing bisphenol AF, dichlorodiphenyl sulfone, N-methylpyrrolidone, anhydrous potassium carbonate and toluene, reacting for 3 hours at the rotation speed of 300r/min and the temperature of 150 ℃, heating to the temperature of 170 ℃, reacting for 4 hours, heating to the temperature of 190 ℃, reacting for 4 hours to obtain an intermediate 1, uniformly mixing the intermediate 1, hydroquinone, anhydrous potassium carbonate and toluene, reacting for 3 hours at the rotation speed of 300r/min and the temperature of 150 ℃, heating to the temperature of 170 ℃, reacting for 4 hours, heating to the temperature of 190 ℃, and reacting for 4 hours to obtain an intermediate 2;
step A2: uniformly mixing the intermediate 2, epichlorohydrin and benzyltriethylammonium chloride, reacting for 4 hours at the rotation speed of 300r/min and the temperature of 90 ℃, adding a sodium hydroxide solution, continuing to react for 1.5 hours to prepare epoxy resin, adding aluminum trichloride and carbon tetrachloride into a reaction kettle, stirring and adding nitrobenzene under the conditions of 200r/min and 15 ℃, reacting for 1.5 hours at the temperature of 45 ℃, filtering to remove filter residue, distilling and dissolving filtrate, mixing a substrate and deionized water, and refluxing for 15 minutes at the temperature of 120 ℃ to prepare an intermediate 3;
step A3: uniformly mixing tin powder, the intermediate 3 and concentrated hydrochloric acid, reacting for 40min at the rotation speed of 200r/min and the temperature of 100 ℃, adjusting the pH value of a reaction solution to be 11 to obtain an intermediate 4, uniformly mixing the intermediate 4, triethylamine and toluene, stirring and introducing triphosgene at the rotation speed of 300r/min and the temperature of 50 ℃ to react for 5h to obtain an intermediate 5, uniformly mixing the intermediate 5, deionized water, ethanol and sodium borohydride, reacting for 40min at the rotation speed of 300r/min and the temperature of 25 ℃, adding a hydrochloric acid solution, and uniformly mixing to obtain an intermediate 6;
step A4: uniformly mixing the intermediate 6, bromooctadecane, sodium hydroxide and N, N-dimethylformamide, reacting for 8 hours at the rotation speed of 200r/min and the temperature of 70 ℃ to obtain an intermediate 7, uniformly mixing the intermediate 7 and epoxy resin, introducing nitrogen for protection, reacting for 1.5 hours at the temperature of 120 ℃, adding dibutyltin dilaurate, and continuously reacting for 1.5 hours to obtain the modified resin.
Comparative example 1
This comparative example compared with example 1, the same procedure was followed except that epoxy resin E-44 was used in place of the modified epoxy resin.
Comparative example 2
The comparative example is a waterproof fabric disclosed in Chinese patent CN 109760397A.
Comparative example 3
The comparative example is a waterproof fabric disclosed in Chinese patent CN 110067132A.
The waterproof fabrics prepared in examples 1 to 3 and comparative examples 1 to 3 were tested according to the standard of ATCC-22-2017, and the spraying method: the water temperature is 27 ℃; washing procedure: the test sample is subjected to routine washing, hanging and airing at the temperature of 27 ℃, is washed for 20 times, is folded in half for 200 times, and the waterproof effect of the folded part is detected, and the results are shown in the following table;
| example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Waterproof/minute | 100 | 100 | 100 | 100 | 100 | 100 |
| Water-proof for 20 times of washing | 100 | 100 | 100 | 80 | 90 | 80 |
| Folding 200 times for water-proof/min | 100 | 100 | 100 | 50 | 70 | 70 |
From the above table, it can be seen that the waterproof value of the waterproof fabric prepared in the embodiments 1 to 3 is 100, and the waterproof value is still 100 after the waterproof fabric is washed 20 times and folded 200 times.
The foregoing is illustrative and explanatory only of the present invention, and it is intended that the present invention cover modifications, additions, or substitutions by those skilled in the art, without departing from the spirit of the invention or exceeding the scope of the claims.
Claims (6)
1. The high stain-resistant waterproof fabric is characterized in that: soaking the fabric base material in modified resin, and curing to obtain the fabric;
the modified resin is prepared by the following steps:
step A1: mixing bisphenol AF, dichlorodiphenyl sulfone, N-methylpyrrolidone, anhydrous potassium carbonate and toluene for reaction, heating for continuous reaction, heating for reaction again to obtain an intermediate 1, mixing the intermediate 1, hydroquinone, anhydrous potassium carbonate and toluene for reaction, heating for continuous reaction, and heating for reaction again to obtain an intermediate 2;
step A2: mixing the intermediate 2, epichlorohydrin and benzyltriethylammonium chloride for heating reaction, adding a sodium hydroxide solution, continuing the reaction to obtain epoxy resin, mixing and stirring aluminum trichloride and carbon tetrachloride, adding nitrobenzene, filtering to remove filter residue, distilling and dissolving the filtrate, mixing a substrate and deionized water, and performing reflux treatment to obtain an intermediate 3;
step A3: mixing tin powder, the intermediate 3 and concentrated hydrochloric acid for reaction, adjusting the pH value of a reaction solution to obtain an intermediate 4, mixing and stirring the intermediate 4, triethylamine and toluene, introducing triphosgene for reaction to obtain an intermediate 5, mixing and reacting the intermediate 5, deionized water, ethanol and sodium borohydride, adding a hydrochloric acid solution, and uniformly mixing to obtain an intermediate 6;
step A4: mixing the intermediate 6, bromooctadecane, sodium hydroxide and N, N-dimethylformamide for reaction to prepare an intermediate 7, mixing the intermediate 7 with epoxy resin for reaction h, adding dibutyl tin dilaurate for continuous reaction to prepare the modified resin.
2. The high stain-resistant waterproof fabric according to claim 1, wherein: the molar ratio of the used bisphenol AF and the used dichlorodiphenyl sulfone in the step A1 is 0.98:1, and the molar ratio of the used intermediate 1 and hydroquinone is 1:2.
3. The high stain-resistant waterproof fabric according to claim 1, wherein: the intermediate 2, the epichlorohydrin, the benzyltriethylammonium chloride and the sodium hydroxide solution in the step A2 are used in a dosage ratio of 0.01mol to 0.02mol to 10.2mg to 50mL, the mass fraction of the sodium hydroxide solution is 25%, the dosage molar ratio of the aluminum trichloride to the carbon tetrachloride is 2:1, and the dosage ratio of the substrate to the deionized water is 1g to 5 mL.
4. The high stain-resistant waterproof fabric according to claim 1, wherein: the using amount ratio of the tin powder, the intermediate 3 and the concentrated hydrochloric acid in the step A3 is 9g:0.01mol:20mL, the mass fraction of the concentrated hydrochloric acid is 36%, the using amount molar ratio of the intermediate 4 and the triphosgene is 1:2.1, the using amount ratio of the intermediate 5, the deionized water, the ethanol, the sodium borohydride and the hydrochloric acid solution is 0.05mol:5mL:20mL:0.5g:2mL, and the mass fraction of the hydrochloric acid solution is 5%.
5. The high stain-resistant waterproof fabric according to claim 1, wherein: the molar ratio of the intermediate 6, bromooctadecane and sodium hydroxide in the step A4 is 1:1:1, and the molar ratio of the intermediate 7, the epoxy resin and the dibutyl tin dilaurate is 0.03mol:0.01mol:0.2 mL.
6. The preparation process of the high stain-resistant waterproof fabric according to claim 1, characterized in that: the method specifically comprises the following steps:
step S1: soaking the fabric base material in modified resin, and performing ultrasonic treatment for 3-5h at the temperature of 70-80 ℃ and the frequency of 50-60 kHz;
step S2: adding diethylenetriamine into the epoxy resin, and carrying out ultrasonic treatment for 30-40min under the condition that the frequency is 70-80 kHz;
step S3: taking out the fabric base material, vertically hanging until no liquid drips, and drying at the temperature of 30-50 ℃ to obtain the high stain-resistant waterproof fabric.
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| CN202111586285.8A CN114645458A (en) | 2021-12-23 | 2021-12-23 | High-stain-resistance waterproof fabric and preparation process thereof |
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| CN202111586285.8A CN114645458A (en) | 2021-12-23 | 2021-12-23 | High-stain-resistance waterproof fabric and preparation process thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115558397A (en) * | 2022-07-26 | 2023-01-03 | 蚌埠朋邦建筑劳务有限公司 | High-durability exterior wall coating and preparation method thereof |
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2021
- 2021-12-23 CN CN202111586285.8A patent/CN114645458A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115558397A (en) * | 2022-07-26 | 2023-01-03 | 蚌埠朋邦建筑劳务有限公司 | High-durability exterior wall coating and preparation method thereof |
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Application publication date: 20220621 |