Highly waterproof polyester fabric and heat preservation bag made of highly waterproof polyester fabric
By preparing antibacterial waterproof lotion and modifying the polyester fabric, the problem of insulating bags being easily contaminated during use is solved, and the high waterproof and antibacterial performance is improved.
Patent Information
- Application Number
- CN202411733175.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-29
- Publication Date
- 2025-03-11
AI Technical Summary
During use, existing insulation bags are susceptible to damage and contamination by food and other substances, making it difficult to solve hygiene problems.
By preparing an antibacterial waterproof emulsion, the antibacterial waterproof modifier is dispersed into deionized water, and non-ionic and cationic surfactants are added for emulsion, then the polyester fabric is immersed in the emulsion and ultraviolet radiation is applied, and finally washed and dried to prepare a highly waterproof polyester fabric.
It improves the waterproof and antibacterial properties of polyester fabrics, enhances its resistance to water vapor and pollution, extends the waterproof effect and maintains antibacterial activity.
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Figure BDA0005160812460000111
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of polyester fabrics, in particular to a highly waterproof polyester fabric and a heat preservation bag prepared therefrom. Background Art
[0002] Insulation bag is a kind of bag used for product packaging and delivery. It is often used for the storage and transportation of food and other items that need to be kept warm.
[0003] Existing insulation bags are generally made of fiber cloth as the outer shell and composite insulation materials in the middle. However, when the insulation bag is working, since it often needs to deal with the storage of food and other various objects that need to be insulated, it is inevitable that food and other materials will be damaged in this process, causing the surface of the insulation bag to be contaminated, making the hygiene of the insulation bag a difficult problem to solve. Summary of the invention
[0004] The purpose of the present invention is to provide a highly waterproof polyester fabric and a heat preservation bag prepared therefrom, so as to solve the problems raised in the prior art.
[0005] To achieve the above object, the present invention provides the following technical solution: a method for preparing a highly waterproof polyester fabric, comprising the following steps:
[0006] S1. preparing antibacterial and waterproof emulsion;
[0007] Dispersing the antibacterial and waterproof modifier prepared in step S1 into deionized water, adding a nonionic surfactant and a cationic surfactant, and stirring at high speed for 30-90 minutes to emulsify to obtain an antibacterial and waterproof emulsion;
[0008] S2. Preparation of highly waterproof polyester fabric;
[0009] After washing and drying the polyester fabric, it is completely immersed in the antibacterial and waterproof emulsion and irradiated with ultraviolet light. After the irradiation, the polyester fabric is taken out, washed with anhydrous ethanol and acetone for 2-3 times respectively, and dried to constant weight to obtain a highly waterproof polyester fabric.
[0010] Furthermore, in step S1, the preparation method of the antibacterial and waterproof modifier is:
[0011] S11. Under nitrogen atmosphere, hydrochloric acid was added dropwise to deionized water to adjust the pH value to 3.5-5, and zinc chloride was added. After stirring and dispersing evenly, 2-acrylic acid-2-carboxyethyl ester was dispersed in deionized water, and stirring and mixing was continued for 5-15 minutes. Then, 2,2,2-trifluoroethanol was added thereto, and the temperature was raised to 75-77° C., and stirred and refluxed for 2-4 hours. After removing excess solvent by rotary evaporation, an acrylate intermediate was obtained;
[0012] S12. Disperse 2-vinyl-4,6-diamino-1,3,5-triazine in DMF, protect under nitrogen atmosphere, disperse uniformly by ultrasonication, add hydrochloric acid, adjust the pH value of the system to 3-5, add dicyandiamide, heat to 90-120° C., stir and react for 0.5-4 h, remove excess solvent by rotary evaporation, wash the reaction product with deionized water 2-3 times, and vacuum dry to constant weight to obtain a vinylguanidine intermediate;
[0013] S13. The vinylguanidine intermediate obtained in step S22 is dispersed in pure DMF, stirred and mixed for 15-30 min, cooled to a constant temperature in an ice-water bath, potassium persulfate is added thereto, and mixing is continued for 1-3 min to obtain a vinylguanidine intermediate dispersion for standby use;
[0014] The acrylate intermediate obtained in step S11 is dispersed in DMF, stirred for 15-20 minutes, and then a polymerization inhibitor is added. After mixing for 1-3 minutes, the temperature is raised to 80-90° C., and 50% of the vinylguanidine intermediate dispersion is uniformly added thereto within 1-2 hours. After the addition is completed, the mixture is stirred for reaction for 0.5 hours, and the remaining vinylguanidine intermediate dispersion is slowly added thereto within 1-2 hours. After the addition is completed, the mixture is reacted for 0.5-1 hours, and the excess solvent is removed by rotary evaporation. The product is washed with deionized water for 2-4 times, and then dried to constant weight to obtain an antibacterial modified intermediate;
[0015] S14. The antibacterial modified intermediate is dispersed in DMF, protected by nitrogen atmosphere, heated to 45-55°C, stirred for 1-2 hours, and then benzophenone-4,4-dicarboxylic acid is added thereto. The temperature is raised to 120-130°C, stirred for reaction for 8-24 hours, and then the excess solvent is removed by rotary evaporation to obtain an antibacterial and waterproof modifier.
[0016] Furthermore, in step S11, the mass ratio of zinc chloride, 2-carboxyethyl 2-acrylate, and 2,2,2-trifluoroethanol is (0.001-0.01):1:(0.61-0.7).
[0017] Furthermore, in step S12, the mass ratio of 2-vinyl-4,6-diamino-1,3,5-triazine to dicyandiamide is 1:(0.9-1.3).
[0018] Further, in step S13, the mass ratio of the vinylguanidine intermediate, potassium persulfate, and acrylate intermediate is 1:(0.001-0.003):(0.65-0.85);
[0019] The mass ratio of the vinylguanidine intermediate to the polymerization inhibitor is 1:(0.03-0.05);
[0020] The polymerization inhibitor is resorcinol.
[0021] Furthermore, in step S14, the mass ratio of the antibacterial modified intermediate and benzophenone-4,4-dicarboxylic acid is (3-4):1.
[0022] Furthermore, in step S1, the antibacterial waterproof emulsion is composed of 15-25 parts of antibacterial waterproof modifier, 0.5-0.8 parts of nonionic surfactant, 1.5-2 parts of cationic surfactant and 130 parts of deionized water in parts by weight.
[0023] Furthermore, in step S2, during ultraviolet irradiation, the irradiation power is 300-700W, the irradiation distance is 15-30cm, and the irradiation time is 15-30min.
[0024] Furthermore, a highly waterproof polyester fabric is prepared by the above method;
[0025] Furthermore, a heat preservation bag is made of the above-mentioned highly waterproof polyester fabric, and a temperature sensor is provided in the heat preservation bag to detect the internal temperature of the heat preservation bag. When the detected temperature is greater than 80°C, the temperature sensor will issue an alarm.
[0026] Compared with the prior art, the present invention has the following beneficial effects:
[0027] In order to improve the pollution resistance and sanitation of the thermal insulation bag, the present invention performs a modification treatment on the polyester fabric of the thermal insulation bag, and finishes the polyester fabric with an antibacterial and waterproof emulsion, so that the polyester fabric has waterproof, hydrophobic and antibacterial functions;
[0028] When preparing the antibacterial waterproof emulsion, the present invention first uses 2,2,2-trifluoroethanol as a raw material to react with 2-acrylic acid-2-carboxyethyl ester containing a propylene double bond and a carboxyl group, and utilizes the reaction between the alcohol hydroxyl group and the carboxyl group to prepare an acrylate intermediate containing a fluorine element and a propylene double bond;
[0029] Then, the present invention further uses 2-vinyl-4,6-diamino-1,3,5-triazine containing a triazine ring and an amino group to react with dicyandiamide containing a cyanide bond, and utilizes the reaction between the cyano group and the amino group to continue to introduce a grafted guanidine group with antibacterial function on the basis of the triazine ring structure. Then, under the action of an initiator, the vinylguanidine intermediate and the acrylate intermediate are mixed and reacted, and the double bonds between them are cross-linked to combine the fluorine element and the guanidine group, and finally an antibacterial modified intermediate is prepared; the fluorine element contained therein can effectively reduce the surface energy of the polyester fabric, enhance the surface hydrophobic effect of the material, avoid the penetration and erosion of water vapor, thereby achieving a waterproof function, and on the basis of avoiding stains, it can also effectively prevent external rain and other water vapor from penetrating the fabric to cause pollution to the items in the insulation bag; and the triazine ring and guanidine structure introduced in this process have excellent antibacterial activity, which can effectively avoid the growth and pollution of pathogenic bacteria and maintain the hygiene and safety of the insulation bag;
[0030] On this basis, the present invention further uses benzophenone-4,4-dicarboxylic acid containing a carboxyl group to react with an antibacterial modified intermediate, and utilizes the reaction between the amino group and the carboxyl group to further introduce a photoreactive benzophenone structure into the antibacterial waterproof emulsion. Afterwards, under ultraviolet irradiation, the benzophenone group reacts with the methylene group in the polyester fiber, thereby grafting the antibacterial modified intermediate onto the surface of the polyester fiber, thereby effectively avoiding the problem of failure of the waterproof effect and decreased antibacterial activity caused by repeated washing. DETAILED DESCRIPTION
[0031] Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative work shall fall within the scope of protection of the present invention.
[0032] The polyester fabric used in this application is a plain weave fabric with a grammage of 85g / m 2 ;
[0033] Embodiment 1. A method for preparing a highly waterproof polyester fabric, comprising the following steps:
[0034] S1. preparing antibacterial and waterproof emulsion;
[0035] Disperse 15 parts of the antibacterial and waterproof modifier prepared in step S1 into 130 parts of deionized water by weight, add 0.5 parts of nonionic surfactant and 1.6 parts of cationic surfactant, and stir at high speed for 80 minutes to obtain an antibacterial and waterproof emulsion;
[0036] Wherein, the preparation method of the antibacterial and waterproof modifier is:
[0037] S11. Under nitrogen atmosphere, hydrochloric acid was added dropwise to deionized water to adjust the pH value to 4, and then 0.01 parts of zinc chloride were added. After stirring and dispersing evenly, 1 part of 2-acrylic acid-2-carboxyethyl ester was dispersed in deionized water. After stirring and mixing for 15 minutes, 0.61 parts of 2,2,2-trifluoroethanol were added thereto. The temperature was raised to 75-77° C., and the reaction was stirred and refluxed for 3 hours. After the excess solvent was removed by rotary evaporation, an acrylate intermediate was obtained.
[0038] S12. Disperse 1 part of 2-vinyl-4,6-diamino-1,3,5-triazine in DMF by weight, protect under nitrogen atmosphere, disperse evenly by ultrasonication, add hydrochloric acid, adjust the pH value of the system to 4, add 0.9 parts of dicyandiamide, heat to 103°C, stir to react for 2.5h, remove excess solvent by rotary evaporation, wash the reaction product twice with deionized water, and vacuum dry to constant weight to obtain a vinylguanidine intermediate;
[0039] S13. In parts by weight, 1 part of the vinylguanidine intermediate obtained in step S22 was dispersed in pure DMF, stirred and mixed for 15 min, cooled to a constant temperature in an ice-water bath, and 0.002 parts of potassium persulfate were added thereto, and mixing was continued for 2 min to obtain a dispersion of the vinylguanidine intermediate for later use;
[0040] Disperse 0.65 parts of the acrylate intermediate obtained in step S11 into DMF, stir for 15 minutes, add 0.05 parts of a resorcinol inhibitor, continue mixing for 2 minutes, raise the temperature to 87°C, uniformly dropwise add 50% of the vinylguanidine intermediate dispersion within 1.5 hours, stir and react for 0.5 hours after the dropwise addition, slowly dropwise add the remaining vinylguanidine intermediate dispersion within 1 hour, continue to react for 1 hour after the dropwise addition, remove excess solvent by rotary evaporation, wash the product with deionized water 3 times, and dry to constant weight to obtain an antibacterial modified intermediate;
[0041] S14. Disperse 3 parts of the antibacterial modified intermediate into DMF by weight, protect under nitrogen atmosphere, heat to 55 ° C, stir for 1 hour, add 1 part of benzophenone-4,4-dicarboxylic acid, heat to 120 ° C, stir for 16 hours, and remove excess solvent by rotary evaporation to obtain an antibacterial waterproof modifier;
[0042] S2. Preparation of highly waterproof polyester fabric;
[0043] After washing and drying the polyester fabric, it was completely immersed in the antibacterial and waterproof emulsion with an immersion depth of 5 mm below the liquid surface. Ultraviolet irradiation was applied externally with an irradiation power of 300 W, an irradiation distance of 15 cm, and an irradiation time of 15 min. After the irradiation, the polyester fabric was taken out, washed three times with anhydrous ethanol and acetone respectively, and dried to constant weight to obtain a highly waterproof polyester fabric.
[0044] Embodiment 2. A method for preparing a highly waterproof polyester fabric, comprising the following steps:
[0045] Compared with Example 1, this example increases the amount of 2,2,2-trifluoroethanol added in step S11;
[0046] S11. Under nitrogen atmosphere, hydrochloric acid was added dropwise to deionized water by weight to adjust the pH value to 4, and then 0.01 parts of zinc chloride were added. After stirring and dispersing evenly, 1 part of 2-acrylic acid-2-carboxyethyl ester was dispersed in deionized water, and stirring and mixing was continued for 15 minutes. Then, 0.7 parts of 2,2,2-trifluoroethanol were added thereto, and the temperature was raised to 75-77° C., and the reaction was stirred and refluxed for 3 hours. After the excess solvent was removed by rotary evaporation, an acrylate intermediate was obtained;
[0047] S12. Disperse 1 part of 2-vinyl-4,6-diamino-1,3,5-triazine in DMF by weight, protect under nitrogen atmosphere, disperse evenly by ultrasonication, add hydrochloric acid, adjust the pH value of the system to 4, add 0.9 parts of dicyandiamide, heat to 103°C, stir to react for 2.5h, remove excess solvent by rotary evaporation, wash the reaction product twice with deionized water, and vacuum dry to constant weight to obtain a vinylguanidine intermediate;
[0048] S13. In parts by weight, 1 part of the vinylguanidine intermediate obtained in step S22 was dispersed in pure DMF, stirred and mixed for 15 min, cooled to a constant temperature in an ice-water bath, and 0.002 parts of potassium persulfate were added thereto, and mixing was continued for 2 min to obtain a dispersion of the vinylguanidine intermediate for later use;
[0049] Disperse 0.65 parts of the acrylate intermediate obtained in step S11 into DMF, stir for 15 minutes, add 0.05 parts of a resorcinol inhibitor, continue mixing for 2 minutes, raise the temperature to 87°C, uniformly dropwise add 50% of the vinylguanidine intermediate dispersion within 1.5 hours, stir and react for 0.5 hours after the dropwise addition, slowly dropwise add the remaining vinylguanidine intermediate dispersion within 1 hour, continue to react for 1 hour after the dropwise addition, remove excess solvent by rotary evaporation, wash the product with deionized water 3 times, and dry to constant weight to obtain an antibacterial modified intermediate;
[0050] S14. Disperse 3 parts of the antibacterial modified intermediate into DMF by weight, protect under nitrogen atmosphere, heat to 55°C, stir for 1 hour, add 1 part of benzophenone-4,4-dicarboxylic acid, heat to 120°C, stir for 16 hours, and remove excess solvent by rotary evaporation to obtain an antibacterial and waterproof modifier.
[0051] Embodiment 3. A method for preparing a highly waterproof polyester fabric, comprising the following steps:
[0052] Compared with Example 2, this embodiment increases the amount of dicyandiamide added in step S12;
[0053] S11. Under nitrogen atmosphere, hydrochloric acid was added dropwise to deionized water by weight to adjust the pH value to 4, and then 0.01 parts of zinc chloride were added. After stirring and dispersing evenly, 1 part of 2-acrylic acid-2-carboxyethyl ester was dispersed in deionized water, and stirring and mixing was continued for 15 minutes. Then, 0.7 parts of 2,2,2-trifluoroethanol were added thereto, and the temperature was raised to 75-77° C., and the reaction was stirred and refluxed for 3 hours. After the excess solvent was removed by rotary evaporation, an acrylate intermediate was obtained;
[0054] S12. Disperse 1 part of 2-vinyl-4,6-diamino-1,3,5-triazine in DMF by weight, protect under nitrogen atmosphere, disperse evenly by ultrasonication, add hydrochloric acid, adjust the pH value of the system to 4, add 1.3 parts of dicyandiamide, heat to 103°C, stir and react for 2.5h, remove excess solvent by rotary evaporation, wash the reaction product twice with deionized water, and vacuum dry to constant weight to obtain a vinylguanidine intermediate;
[0055] S13. In parts by weight, 1 part of the vinylguanidine intermediate obtained in step S22 was dispersed in pure DMF, stirred and mixed for 15 min, cooled to a constant temperature in an ice-water bath, and 0.002 parts of potassium persulfate were added thereto, and mixing was continued for 2 min to obtain a dispersion of the vinylguanidine intermediate for later use;
[0056] Disperse 0.65 parts of the acrylate intermediate obtained in step S11 into DMF, stir for 15 minutes, add 0.05 parts of a resorcinol inhibitor, continue mixing for 2 minutes, raise the temperature to 87°C, uniformly dropwise add 50% of the vinylguanidine intermediate dispersion within 1.5 hours, stir and react for 0.5 hours after the dropwise addition, slowly dropwise add the remaining vinylguanidine intermediate dispersion within 1 hour, continue to react for 1 hour after the dropwise addition, remove excess solvent by rotary evaporation, wash the product with deionized water 3 times, and dry to constant weight to obtain an antibacterial modified intermediate;
[0057] S14. Disperse 3 parts of the antibacterial modified intermediate into DMF by weight, protect under nitrogen atmosphere, heat to 55°C, stir for 1 hour, add 1 part of benzophenone-4,4-dicarboxylic acid, heat to 120°C, stir for 16 hours, and remove excess solvent by rotary evaporation to obtain an antibacterial and waterproof modifier.
[0058] Embodiment 4. A method for preparing a highly waterproof polyester fabric, comprising the following steps:
[0059] Compared with Example 3, this example increases the amount of acrylate intermediate added in step S13;
[0060] S11. Under nitrogen atmosphere, hydrochloric acid was added dropwise to deionized water by weight to adjust the pH value to 4, and then 0.01 parts of zinc chloride were added. After stirring and dispersing evenly, 1 part of 2-acrylic acid-2-carboxyethyl ester was dispersed in deionized water, and stirring and mixing was continued for 15 minutes. Then, 0.7 parts of 2,2,2-trifluoroethanol were added thereto, and the temperature was raised to 75-77° C., and the reaction was stirred and refluxed for 3 hours. After the excess solvent was removed by rotary evaporation, an acrylate intermediate was obtained;
[0061] S12. Disperse 1 part of 2-vinyl-4,6-diamino-1,3,5-triazine in DMF by weight, protect under nitrogen atmosphere, disperse evenly by ultrasonication, add hydrochloric acid, adjust the pH value of the system to 4, add 1.3 parts of dicyandiamide, heat to 103°C, stir and react for 2.5h, remove excess solvent by rotary evaporation, wash the reaction product twice with deionized water, and vacuum dry to constant weight to obtain a vinylguanidine intermediate;
[0062] S13. In parts by weight, 1 part of the vinylguanidine intermediate obtained in step S22 was dispersed in pure DMF, stirred and mixed for 15 min, cooled to a constant temperature in an ice-water bath, and 0.002 parts of potassium persulfate were added thereto, and mixing was continued for 2 min to obtain a dispersion of the vinylguanidine intermediate for later use;
[0063] Disperse 0.85 parts of the acrylate intermediate obtained in step S11 into DMF, stir for 15 minutes, add 0.05 parts of a resorcinol inhibitor, continue mixing for 2 minutes, heat to 87°C, uniformly dropwise add 50% of the vinylguanidine intermediate dispersion within 1.5 hours, stir and react for 0.5 hours after the dropwise addition, slowly dropwise add the remaining vinylguanidine intermediate dispersion within 1 hour, continue to react for 1 hour after the dropwise addition, remove excess solvent by rotary evaporation, wash the product with deionized water 3 times, and dry to constant weight to obtain an antibacterial modified intermediate;
[0064] S14. Disperse 3 parts of the antibacterial modified intermediate into DMF by weight, protect under nitrogen atmosphere, heat to 55°C, stir for 1 hour, add 1 part of benzophenone-4,4-dicarboxylic acid, heat to 120°C, stir for 16 hours, and remove excess solvent by rotary evaporation to obtain an antibacterial and waterproof modifier.
[0065] Embodiment 5. A method for preparing a highly waterproof polyester fabric, comprising the following steps:
[0066] Compared with Example 4, this example increases the amount of antibacterial modified intermediate added in step S14;
[0067] S11. Under nitrogen atmosphere, hydrochloric acid was added dropwise to deionized water by weight to adjust the pH value to 4, and then 0.01 parts of zinc chloride were added. After stirring and dispersing evenly, 1 part of 2-acrylic acid-2-carboxyethyl ester was dispersed in deionized water, and stirring and mixing was continued for 15 minutes. Then, 0.7 parts of 2,2,2-trifluoroethanol were added thereto, and the temperature was raised to 75-77° C., and the reaction was stirred and refluxed for 3 hours. After the excess solvent was removed by rotary evaporation, an acrylate intermediate was obtained;
[0068] S12. Disperse 1 part of 2-vinyl-4,6-diamino-1,3,5-triazine in DMF by weight, protect under nitrogen atmosphere, disperse evenly by ultrasonication, add hydrochloric acid, adjust the pH value of the system to 4, add 1.3 parts of dicyandiamide, heat to 103°C, stir and react for 2.5h, remove excess solvent by rotary evaporation, wash the reaction product twice with deionized water, and vacuum dry to constant weight to obtain a vinylguanidine intermediate;
[0069] S13. In parts by weight, 1 part of the vinylguanidine intermediate obtained in step S22 was dispersed in pure DMF, stirred and mixed for 15 min, cooled to a constant temperature in an ice-water bath, and 0.002 parts of potassium persulfate were added thereto, and mixing was continued for 2 min to obtain a dispersion of the vinylguanidine intermediate for later use;
[0070] Disperse 0.85 parts of the acrylate intermediate obtained in step S11 into DMF, stir for 15 minutes, add 0.05 parts of a resorcinol inhibitor, continue mixing for 2 minutes, heat to 87°C, uniformly dropwise add 50% of the vinylguanidine intermediate dispersion within 1.5 hours, stir and react for 0.5 hours after the dropwise addition, slowly dropwise add the remaining vinylguanidine intermediate dispersion within 1 hour, continue to react for 1 hour after the dropwise addition, remove excess solvent by rotary evaporation, wash the product with deionized water 3 times, and dry to constant weight to obtain an antibacterial modified intermediate;
[0071] S14. Disperse 4 parts of the antibacterial modified intermediate into DMF by weight, protect under nitrogen atmosphere, heat to 55°C, stir for 1 hour, add 1 part of benzophenone-4,4-dicarboxylic acid, heat to 120°C, stir for 16 hours, and remove excess solvent by rotary evaporation to obtain an antibacterial and waterproof modifier.
[0072] Embodiment 6. A method for preparing a highly waterproof polyester fabric, comprising the following steps:
[0073] Compared with Example 5, this embodiment increases the amount of antibacterial and waterproof modifier added in step S1;
[0074] S1. preparing antibacterial and waterproof emulsion;
[0075] Disperse 25 parts of the antibacterial and waterproof modifier prepared in step S1 into 130 parts of deionized water by weight, add 0.5 parts of nonionic surfactant and 1.6 parts of cationic surfactant, and stir at high speed for 80 minutes to obtain an antibacterial and waterproof emulsion;
[0076] Wherein, the preparation method of the antibacterial and waterproof modifier is:
[0077] S11. Under nitrogen atmosphere, hydrochloric acid was added dropwise to deionized water by weight to adjust the pH value to 4, and then 0.01 parts of zinc chloride were added. After stirring and dispersing evenly, 1 part of 2-acrylic acid-2-carboxyethyl ester was dispersed in deionized water, and stirring and mixing was continued for 15 minutes. Then, 0.7 parts of 2,2,2-trifluoroethanol were added thereto, and the temperature was raised to 75-77° C., and the reaction was stirred and refluxed for 3 hours. After the excess solvent was removed by rotary evaporation, an acrylate intermediate was obtained;
[0078] S12. Disperse 1 part of 2-vinyl-4,6-diamino-1,3,5-triazine in DMF by weight, protect under nitrogen atmosphere, disperse evenly by ultrasonication, add hydrochloric acid, adjust the pH value of the system to 4, add 1.3 parts of dicyandiamide, heat to 103°C, stir and react for 2.5h, remove excess solvent by rotary evaporation, wash the reaction product twice with deionized water, and vacuum dry to constant weight to obtain a vinylguanidine intermediate;
[0079] S13. In parts by weight, 1 part of the vinylguanidine intermediate obtained in step S22 was dispersed in pure DMF, stirred and mixed for 15 min, cooled to a constant temperature in an ice-water bath, and 0.002 parts of potassium persulfate were added thereto, and mixing was continued for 2 min to obtain a dispersion of the vinylguanidine intermediate for later use;
[0080] Disperse 0.85 parts of the acrylate intermediate obtained in step S11 into DMF, stir for 15 minutes, add 0.05 parts of a resorcinol inhibitor, continue mixing for 2 minutes, heat to 87°C, uniformly dropwise add 50% of the vinylguanidine intermediate dispersion within 1.5 hours, stir and react for 0.5 hours after the dropwise addition, slowly dropwise add the remaining vinylguanidine intermediate dispersion within 1 hour, continue to react for 1 hour after the dropwise addition, remove excess solvent by rotary evaporation, wash the product with deionized water 3 times, and dry to constant weight to obtain an antibacterial modified intermediate;
[0081] S14. Disperse 4 parts of the antibacterial modified intermediate into DMF by weight, protect under nitrogen atmosphere, heat to 55 ° C, stir for 1 hour, add 1 part of benzophenone-4,4-dicarboxylic acid, heat to 120 ° C, stir for 16 hours, and remove excess solvent by rotary evaporation to obtain an antibacterial waterproof modifier;
[0082] S2. Preparation of highly waterproof polyester fabric;
[0083] After washing and drying the polyester fabric, it was completely immersed in the antibacterial and waterproof emulsion with an immersion depth of 5 mm below the liquid surface. Ultraviolet irradiation was applied externally with an irradiation power of 300 W, an irradiation distance of 15 cm, and an irradiation time of 15 min. After the irradiation, the polyester fabric was taken out, washed three times with anhydrous ethanol and acetone respectively, and dried to constant weight to obtain a highly waterproof polyester fabric.
[0084] Comparative Example 1. A method for preparing a highly waterproof polyester fabric, comprising the following steps:
[0085] Compared with Example 1, this comparative example performs step S14 processing;
[0086] S1. preparing antibacterial and waterproof emulsion;
[0087] By weight, 15 parts of the antibacterial modified intermediate prepared in step S1 were dispersed in 130 parts of deionized water, 0.5 parts of a nonionic surfactant and 1.6 parts of a cationic surfactant were added, and the mixture was stirred at high speed for 80 minutes to obtain an antibacterial and waterproof emulsion;
[0088] Wherein, the preparation method of the antibacterial and waterproof modifier is:
[0089] S11. Under nitrogen atmosphere, hydrochloric acid was added dropwise to deionized water to adjust the pH value to 4, and then 0.01 parts of zinc chloride were added. After stirring and dispersing evenly, 1 part of 2-acrylic acid-2-carboxyethyl ester was dispersed in deionized water. After stirring and mixing for 15 minutes, 0.61 parts of 2,2,2-trifluoroethanol were added thereto. The temperature was raised to 75-77° C., and the reaction was stirred and refluxed for 3 hours. After the excess solvent was removed by rotary evaporation, an acrylate intermediate was obtained.
[0090] S12. Disperse 1 part of 2-vinyl-4,6-diamino-1,3,5-triazine in DMF by weight, protect under nitrogen atmosphere, disperse evenly by ultrasonication, add hydrochloric acid, adjust the pH value of the system to 4, add 0.9 parts of dicyandiamide, heat to 103°C, stir to react for 2.5h, remove excess solvent by rotary evaporation, wash the reaction product twice with deionized water, and vacuum dry to constant weight to obtain a vinylguanidine intermediate;
[0091] S13. In parts by weight, 1 part of the vinylguanidine intermediate obtained in step S22 was dispersed in pure DMF, stirred and mixed for 15 min, cooled to a constant temperature in an ice-water bath, and 0.002 parts of potassium persulfate were added thereto, and mixing was continued for 2 min to obtain a dispersion of the vinylguanidine intermediate for later use;
[0092] Disperse 0.65 parts of the acrylate intermediate obtained in step S11 into DMF, stir for 15 minutes, add 0.05 parts of a resorcinol inhibitor, continue mixing for 2 minutes, raise the temperature to 87°C, uniformly dropwise add 50% of the vinylguanidine intermediate dispersion within 1.5 hours, stir and react for 0.5 hours after the dropwise addition, slowly dropwise add the remaining vinylguanidine intermediate dispersion within 1 hour, continue to react for 1 hour after the dropwise addition, remove excess solvent by rotary evaporation, wash the product with deionized water 3 times, and dry to constant weight to obtain an antibacterial modified intermediate;
[0093] S2. Preparation of highly waterproof polyester fabric;
[0094] After washing and drying the polyester fabric, it was completely immersed in the antibacterial and waterproof emulsion with an immersion depth of 5 mm below the liquid surface. Ultraviolet irradiation was applied externally with an irradiation power of 300 W, an irradiation distance of 15 cm, and an irradiation time of 15 min. After the irradiation, the polyester fabric was taken out, washed three times with anhydrous ethanol and acetone respectively, and dried to constant weight to obtain a highly waterproof polyester fabric.
[0095] Detection:
[0096] The water drop contact angle of the highly waterproof polyester fabrics prepared in Examples 1-6 and Comparative Example 1 was tested using a water drop contact angle measuring instrument;
[0097] According to GB / T 5454-1997, the oxygen index performance of the highly waterproof polyester fabrics prepared in Examples 1-6 and Comparative Example 1 was tested;
[0098] The antibacterial effect of the highly waterproof polyester fabrics prepared in Examples 1-6 and Comparative Example 1 was tested according to the oscillation method in the FZ / T73023 standard;
[0099] The highly waterproof polyester fabrics prepared in Examples 1-6 and Comparative Example 1 were washed 50 times in warm water at 25°C for 30 minutes;
[0100] After washing, the water drop contact angle test, oxygen index performance test and antibacterial effect test were performed again; the test results are shown in the table below;
[0101]
[0102] Finally, it should be noted that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art can still modify the technical solutions described in the aforementioned embodiments or replace some of the technical features therein by equivalents. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.
Claims
1. A method for preparing a highly waterproof polyester fabric, characterized in that: The following steps are involved: S1. preparing antibacterial and waterproof emulsion; Dispersing the antibacterial and waterproof modifier prepared in step S1 into deionized water, adding a nonionic surfactant and a cationic surfactant, and stirring at high speed for 30-90 minutes to emulsify to obtain an antibacterial and waterproof emulsion; S2. Preparation of highly waterproof polyester fabric; After washing and drying the polyester fabric, it is completely immersed in the antibacterial and waterproof emulsion and irradiated with ultraviolet light. After the irradiation, the polyester fabric is taken out, washed with anhydrous ethanol and acetone for 2-3 times respectively, and dried to constant weight to obtain a highly waterproof polyester fabric.
2. The method for preparing a highly waterproof polyester fabric according to claim 1, characterized in that: In step S1, the preparation method of the antibacterial and waterproof modifier is: S11. Under nitrogen atmosphere, hydrochloric acid was added dropwise to deionized water to adjust the pH value to 3.5-5, and zinc chloride was added. After stirring and dispersing evenly, 2-acrylic acid-2-carboxyethyl ester was dispersed in deionized water, and stirring and mixing was continued for 5-15 minutes. Then, 2,2,2-trifluoroethanol was added thereto, and the temperature was raised to 75-77° C., and stirred and refluxed for 2-4 hours. After removing excess solvent by rotary evaporation, an acrylate intermediate was obtained; S12. Disperse 2-vinyl-4,6-diamino-1,3,5-triazine in DMF, protect under nitrogen atmosphere, disperse uniformly by ultrasonication, add hydrochloric acid, adjust the pH value of the system to 3-5, add dicyandiamide, heat to 90-120° C., stir and react for 0.5-4 h, remove excess solvent by rotary evaporation, wash the reaction product with deionized water 2-3 times, and vacuum dry to constant weight to obtain a vinylguanidine intermediate; S13. The vinylguanidine intermediate obtained in step S22 is dispersed in pure DMF, stirred and mixed for 15-30 min, cooled to a constant temperature in an ice-water bath, potassium persulfate is added thereto, and mixing is continued for 1-3 min to obtain a vinylguanidine intermediate dispersion for standby use; The acrylate intermediate obtained in step S11 is dispersed in DMF, stirred for 15-20 minutes, and then a polymerization inhibitor is added. After mixing for 1-3 minutes, the temperature is raised to 80-90° C., and 50% of the vinylguanidine intermediate dispersion is uniformly added thereto within 1-2 hours. After the addition is completed, the mixture is stirred for reaction for 0.5 hours, and the remaining vinylguanidine intermediate dispersion is slowly added thereto within 1-2 hours. After the addition is completed, the mixture is reacted for 0.5-1 hours, and the excess solvent is removed by rotary evaporation. The product is washed with deionized water for 2-4 times, and then dried to constant weight to obtain an antibacterial modified intermediate; S14. The antibacterial modified intermediate is dispersed in DMF, protected by nitrogen atmosphere, heated to 45-55°C, stirred for 1-2 hours, and then benzophenone-4,4-dicarboxylic acid is added thereto. The temperature is raised to 120-130°C, stirred for reaction for 8-24 hours, and then the excess solvent is removed by rotary evaporation to obtain an antibacterial and waterproof modifier.
3. The method for preparing a highly waterproof polyester fabric according to claim 2, characterized in that: In step S11, the mass ratio of zinc chloride, 2-carboxyethyl 2-acrylate, and 2,2,2-trifluoroethanol is (0.001-0.01):1:(0.61-0.7).
4. The method for preparing a highly waterproof polyester fabric according to claim 2, characterized in that: In step S12, the mass ratio of 2-vinyl-4,6-diamino-1,3,5-triazine to dicyandiamide is 1:(0.9-1.3).
5. The method for preparing a highly waterproof polyester fabric according to claim 2, characterized in that: In step S13, the mass ratio of the vinylguanidine intermediate, potassium persulfate, and acrylate intermediate is 1:(0.001-0.003):(0.65-0.85); The mass ratio of the vinylguanidine intermediate to the polymerization inhibitor is 1:(0.03-0.05); The polymerization inhibitor is resorcinol.
6. The method for preparing a highly waterproof polyester fabric according to claim 2, characterized in that: In step S14, the mass ratio of the antibacterial modified intermediate and benzophenone-4,4-dicarboxylic acid is (3-4):
1.
7. The method for preparing a highly waterproof polyester fabric according to claim 1, characterized in that: In step S1, the antibacterial waterproof emulsion is composed of 15-25 parts of antibacterial waterproof modifier, 0.5-0.8 parts of nonionic surfactant, 1.5-2 parts of cationic surfactant and 130 parts of deionized water in parts by weight.
8. The method for preparing a highly waterproof polyester fabric according to claim 1, characterized in that: In step S2, during ultraviolet irradiation, the irradiation power is 300-700W, the irradiation distance is 15-30cm, and the irradiation time is 15-30min.
9. A highly waterproof polyester fabric prepared by the preparation method according to any one of claims 1 to 8.
10. A thermal insulation bag made of highly waterproof polyester fabric as claimed in claim 9, characterized in that: The insulation bag is provided with a temperature sensor for detecting the internal temperature of the insulation bag, and an alarm is issued when the detected temperature reaches a preset target temperature.