Antibacterial and uvioresistant polyester master batch and preparation method thereof

Abstract

The invention discloses an antibacterial and anti-ultraviolet polyester master batch and a preparation method thereof, relates to the technical field of polyester resin, and aims to improve the antibacterial performance and the anti-ultraviolet performance of a polyester material, an antibacterial and anti-ultraviolet intermediate is prepared and added into the polyester material; according to the preparation method, a guanidyl structure with antibacterial performance and benzophenone and triazine ring structures with anti-ultraviolet performance are introduced into an antibacterial and anti-ultraviolet intermediate, so that the anti-ultraviolet performance of the antibacterial and anti-ultraviolet intermediate is improved, and the antibacterial and anti-ultraviolet intermediate reacts with ethylene glycol and other raw materials; therefore, an antibacterial and anti-ultraviolet structure is introduced into a polyester chain segment, the antibacterial performance and the anti-ultraviolet performance of polyester are enhanced, and the use performance of a polyester material is improved.

Description

Technical Field

[0001] The invention relates to the technical field of polyester, in particular to an antibacterial and anti-ultraviolet polyester masterbatch and a preparation method thereof. Background Art

[0002] Polyester plastic is a kind of engineering plastic that is safe, non-toxic, has excellent mechanical properties and high chemical stability. It can be widely used in food packaging and medical device packaging. However, during use, polyester materials are not resistant to aging. Under sunlight, polyester plastics will deteriorate in performance and even cause packaging damage, causing the performance of polyester to decline or even fail to achieve its original function. In addition, polyester materials do not have antibacterial properties and are easily infected by bacteria, causing contamination of the packaging. Therefore, it is necessary to improve these defects. Summary of the invention

[0003] The object of the present invention is to provide an antibacterial and anti-ultraviolet polyester masterbatch and a preparation method thereof, so as to solve the problems raised in the prior art.

[0004] To achieve the above object, the present invention provides the following technical solution: a method for preparing an antibacterial and anti-ultraviolet polyester masterbatch, comprising the following steps:

[0005] S1. Preparation of antibacterial and anti-ultraviolet masterbatch;

[0006] S11. Under nitrogen atmosphere protection, 2,4-dihydroxybenzophenone was dispersed in a mixed solvent of acetone and deionized water in a volume ratio of 3:1, and after stirring evenly, sodium hydroxide was added thereto, and the mixture was cooled to a constant temperature in an ice-water bath, and stirred for 2-4 hours, and 3-amino-6-bromo-1,2,4-triazine was added thereto, and the reaction was continued with stirring for 4-8 hours. After removing the excess solvent by rotary evaporation, the product was washed with deionized water at a temperature of 0-5°C, and vacuum dried to constant weight to obtain an aminobenzophenone compound;

[0007] S12. The aminobenzophenone compound is dispersed in acetone, ultrasonically dispersed for 40-80 min, and then cyanamide is added thereto, and the mixture is protected by a nitrogen atmosphere, and the temperature is raised to 55-56° C., and the mixture is refluxed for 12-48 h, and then the excess solvent is removed by rotary evaporation to obtain a guanidinobenzophenone compound;

[0008] S13. Disperse 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine in DMF, protect under nitrogen atmosphere, stir and mix for 15-45 minutes, add 1-ethyl-(3-dimethylaminopropyl)carbodiimide, continue to mix for 3-5 minutes, add guanidinobenzophenone compound, heat to 115-120° C., stir and react for 4-12 hours, and remove excess solvent by rotary evaporation to obtain an antibacterial and anti-ultraviolet intermediate;

[0009] S14. The antibacterial and anti-ultraviolet intermediate is mixed with terephthalic acid, ethylene glycol and butyl titanate are added, and the esterification reaction is continued for 3-5 hours, and trimethyl phosphate is added thereto. After the esterification reaction is continued for 2-4 hours, the heating is stopped and the product is extruded and cooled with cold water, and then pelletized to obtain an antibacterial and anti-ultraviolet masterbatch;

[0010] S2. Mix the PET masterbatch and the antibacterial and anti-ultraviolet masterbatch by weight, melt them at high temperature, extrude and pelletize them to obtain the antibacterial and anti-ultraviolet polyester masterbatch.

[0011] Furthermore, in terms of weight, in step S11, the mass ratio of 2,4-dihydroxybenzophenone, sodium hydroxide, and 3-amino-6-bromo-1,2,4-triazine is 10:(1.5-2):(6-8.2).

[0012] Furthermore, in terms of parts by weight, in step S12, the mass ratio of the aminobenzophenone compound to cyanamide is 10:(0.9-1.1).

[0013] Furthermore, in terms of weight, in step S13, the mass ratio of the 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine, 1-ethyl-(3-dimethylaminopropyl)carbodiimide, and guanidinobenzophenone compound is 10:(0.15-0.2):(8.5-10.2).

[0014] Furthermore, in terms of weight, in step S14, the mass ratio of the antibacterial and anti-ultraviolet intermediate, terephthalic acid, and ethylene glycol is (11-18): (20-24): 12.

[0015] Furthermore, in terms of weight, in step S14, the mass ratio of the antibacterial and anti-ultraviolet intermediate, butyl titanate, and trimethyl phosphate is (11-18): (0.005-0.01): (0.002-0.005).

[0016] Furthermore, in terms of weight, in step S2, the mass ratio of the PET masterbatch to the antibacterial and anti-ultraviolet masterbatch is 10:(3-5).

[0017] Furthermore, in terms of weight, in step S2, the mass ratio of the PET masterbatch to the antibacterial and anti-ultraviolet masterbatch is 10:(3-5).

[0018] Compared with the prior art, the present invention has the following beneficial effects:

[0019] In order to improve the antibacterial and anti-ultraviolet properties of polyester materials, the present invention prepares and adds antibacterial and anti-ultraviolet masterbatch in polyester materials; the present invention first uses 2,4-dihydroxybenzophenone as a raw material, mixes it with sodium hydroxide, uses sodium hydroxide to react with hydroxyl groups in 2,4-dihydroxybenzophenone, and then reacts and grafts it with 3-amino-6-bromo-1,2,4-triazine containing bromine elements, thereby preparing an aminobenzophenone compound with an amino group and a benzophenone structure; wherein benzophenone can effectively absorb UV-B and UV-C rays, convert them into heat energy, and reduce the damage of ultraviolet rays to polyester chain segments;

[0020] On this basis, the present invention uses dicyandiamide to react with an aminobenzophenone compound, utilizes the reaction between an amino group and a cyano group to generate a guanidine group with antibacterial properties, and further reacts the guanidine group with 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine containing a triazine ring structure, thereby preparing an antibacterial and anti-ultraviolet intermediate with a carboxyl terminal group;

[0021] The triazine ring structure has a strong conjugated system, and the π electron cloud formed by the nitrogen atoms and carbon atoms can effectively absorb ultraviolet energy. The electrons in the molecule are excited to a high energy state and converted into heat energy for release, thereby absorbing ultraviolet rays and reducing the damage of ultraviolet rays to polyester. The triazine ring mainly absorbs ultraviolet rays in the UV-A and UV-B regions, and can effectively form a complementary effect with benzophenone, so that the polyester masterbatch prepared by the present invention has anti-ultraviolet performance under multi-band ultraviolet light.

[0022] Afterwards, the present invention also uses antibacterial and anti-ultraviolet intermediates to react with raw materials such as ethylene glycol, thereby introducing antibacterial and anti-ultraviolet structures into the polyester chain segments, enhancing the antibacterial and anti-ultraviolet properties of the polyester and improving the performance of the polyester material. DETAILED DESCRIPTION

[0023] Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in the field without making any creative work shall fall within the scope of protection of the present invention.

[0024] The PET masterbatch used in the present invention is Wankai WK801 polyester chips;

[0025] Embodiment 1. A method for preparing an antibacterial and anti-ultraviolet polyester masterbatch, comprising the following steps:

[0026] S1. Preparation of antibacterial and anti-ultraviolet masterbatch;

[0027] S11. By weight, under nitrogen atmosphere, 10 parts of 2,4-dihydroxybenzophenone were dispersed in a mixed solvent of acetone and deionized water in a volume ratio of 3:1, stirred evenly, and then 2 parts of sodium hydroxide were added thereto. The mixture was cooled to a constant temperature in an ice-water bath, stirred for 3 hours, and then 6 parts of 3-amino-6-bromo-1,2,4-triazine were added thereto. The reaction was continued with stirring for 6 hours, and the excess solvent was removed by rotary evaporation. The product was washed with deionized water at a temperature of 2-4°C, and then vacuum dried to constant weight to obtain an aminobenzophenone compound;

[0028] S12. By weight, 10 parts of an aminobenzophenone compound were dispersed in acetone, and after ultrasonic dispersion for 60 min, 0.9 parts of cyanamide were added thereto, and the mixture was protected by a nitrogen atmosphere, and the temperature was raised to 55-56 ° C. After reflux for 36 h, the excess solvent was removed by rotary evaporation to obtain a guanidinobenzophenone compound;

[0029] S13. Disperse 10 parts of 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine in DMF by weight, protect under nitrogen atmosphere, stir and mix for 30 minutes, add 0.15 parts of 1-ethyl-(3-dimethylaminopropyl)carbodiimide, continue to mix for 3 minutes, add 8.5 parts of guanidine dibenzophenone compound, heat to 115°C, stir and react for 8 hours, and then remove excess solvent by rotary evaporation to obtain an antibacterial and anti-ultraviolet intermediate;

[0030] S14. By weight, 11 parts of the antibacterial and anti-ultraviolet intermediate were mixed with 21 parts of terephthalic acid, 12 parts of ethylene glycol and 0.005 parts of butyl titanate were added, and after esterification for 4 hours, 0.002 trimethyl phosphate was added thereto, and the esterification reaction was continued for 3 hours, and then the heating was stopped and the product was extruded and cooled with cold water, and then pelletized to obtain an antibacterial and anti-ultraviolet masterbatch;

[0031] During the esterification reaction, the reaction temperature was 245°C and the reaction pressure was 0.3MPa;

[0032] S2. Mix 10 parts of PET masterbatch with 3 parts of antibacterial and anti-ultraviolet masterbatch by weight, melt at high temperature, extrude and pelletize to obtain antibacterial and anti-ultraviolet polyester masterbatch.

[0033] Embodiment 2. A method for preparing an antibacterial and anti-ultraviolet polyester masterbatch, comprising the following steps:

[0034] Compared with Example 1, this embodiment increases the amount of antibacterial and anti-ultraviolet masterbatch added in step S2;

[0035] S1. Preparation of antibacterial and anti-ultraviolet masterbatch;

[0036] S11. By weight, under nitrogen atmosphere, 10 parts of 2,4-dihydroxybenzophenone were dispersed in a mixed solvent of acetone and deionized water in a volume ratio of 3:1, stirred evenly, and then 2 parts of sodium hydroxide were added thereto. The mixture was cooled to a constant temperature in an ice-water bath, stirred for 3 hours, and then 6 parts of 3-amino-6-bromo-1,2,4-triazine were added thereto. The reaction was continued with stirring for 6 hours, and the excess solvent was removed by rotary evaporation. The product was washed with deionized water at a temperature of 2-4°C, and then vacuum dried to constant weight to obtain an aminobenzophenone compound;

[0037] S12. By weight, 10 parts of an aminobenzophenone compound were dispersed in acetone, and after ultrasonic dispersion for 60 min, 0.9 parts of cyanamide were added thereto, and the mixture was protected by a nitrogen atmosphere, and the temperature was raised to 55-56 ° C. After reflux for 36 h, the excess solvent was removed by rotary evaporation to obtain a guanidinobenzophenone compound;

[0038] S13. Disperse 10 parts of 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine in DMF by weight, protect under nitrogen atmosphere, stir and mix for 30 minutes, add 0.15 parts of 1-ethyl-(3-dimethylaminopropyl)carbodiimide, continue to mix for 3 minutes, add 8.5 parts of guanidine dibenzophenone compound, heat to 115°C, stir and react for 8 hours, and then remove excess solvent by rotary evaporation to obtain an antibacterial and anti-ultraviolet intermediate;

[0039] S14. By weight, 11 parts of the antibacterial and anti-ultraviolet intermediate were mixed with 21 parts of terephthalic acid, 12 parts of ethylene glycol and 0.005 parts of butyl titanate were added, and after esterification for 4 hours, 0.002 trimethyl phosphate was added thereto, and the esterification reaction was continued for 3 hours, and then the heating was stopped and the product was extruded and cooled with cold water, and then pelletized to obtain an antibacterial and anti-ultraviolet masterbatch;

[0040] During the esterification reaction, the reaction temperature was 245°C and the reaction pressure was 0.3MPa;

[0041] S2. By weight, 10 parts of PET masterbatch and 5 parts of antibacterial and anti-ultraviolet masterbatch are mixed, melted at high temperature, extruded and pelletized to obtain antibacterial and anti-ultraviolet polyester masterbatch.

[0042] Embodiment 3. A method for preparing an antibacterial and anti-ultraviolet polyester masterbatch, comprising the following steps:

[0043] Compared with Example 1, this example increases the amount of 3-amino-6-bromo-1,2,4-triazine added in step S11;

[0044] S1. Preparation of antibacterial and anti-ultraviolet masterbatch;

[0045] S11. According to the weight percentage, under the protection of nitrogen atmosphere, 10 parts of 2,4-dihydroxybenzophenone were dispersed in a mixed solvent of acetone and deionized water in a volume ratio of 3:1, and after stirring evenly, 2 parts of sodium hydroxide were added thereto, and the mixture was cooled to a constant temperature in an ice-water bath, and stirred for 3 hours. Then, 8.2 parts of 3-amino-6-bromo-1,2,4-triazine were added thereto, and the reaction was continued with stirring for 6 hours. After removing the excess solvent by rotary evaporation, the product was washed with deionized water at a temperature of 2-4°C, and vacuum dried to constant weight to obtain an aminobenzophenone compound;

[0046] S12. By weight, 10 parts of an aminobenzophenone compound were dispersed in acetone, and after ultrasonic dispersion for 60 min, 0.9 parts of cyanamide were added thereto, and the mixture was protected by a nitrogen atmosphere, and the temperature was raised to 55-56 ° C. After reflux for 36 h, the excess solvent was removed by rotary evaporation to obtain a guanidinobenzophenone compound;

[0047] S13. Disperse 10 parts of 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine in DMF by weight, protect under nitrogen atmosphere, stir and mix for 30 minutes, add 0.15 parts of 1-ethyl-(3-dimethylaminopropyl)carbodiimide, continue to mix for 3 minutes, add 8.5 parts of guanidine dibenzophenone compound, heat to 115°C, stir and react for 8 hours, and then remove excess solvent by rotary evaporation to obtain an antibacterial and anti-ultraviolet intermediate;

[0048] S14. By weight, 11 parts of the antibacterial and anti-ultraviolet intermediate were mixed with 21 parts of terephthalic acid, 12 parts of ethylene glycol and 0.005 parts of butyl titanate were added, and after esterification for 4 hours, 0.002 trimethyl phosphate was added thereto, and the esterification reaction was continued for 3 hours, and then the heating was stopped and the product was extruded and cooled with cold water, and then pelletized to obtain an antibacterial and anti-ultraviolet masterbatch;

[0049] During the esterification reaction, the reaction temperature was 245°C and the reaction pressure was 0.3MPa;

[0050] S2. Mix 10 parts of PET masterbatch with 3 parts of antibacterial and anti-ultraviolet masterbatch by weight, melt at high temperature, extrude and pelletize to obtain antibacterial and anti-ultraviolet polyester masterbatch.

[0051] Embodiment 4. A method for preparing an antibacterial and anti-ultraviolet polyester masterbatch, comprising the following steps:

[0052] Compared with Example 3, this embodiment increases the amount of cyanamide added in step S12;

[0053] S1. Preparation of antibacterial and anti-ultraviolet masterbatch;

[0054] S11. According to the weight percentage, under the protection of nitrogen atmosphere, 10 parts of 2,4-dihydroxybenzophenone were dispersed in a mixed solvent of acetone and deionized water in a volume ratio of 3:1, and after stirring evenly, 2 parts of sodium hydroxide were added thereto, and the mixture was cooled to a constant temperature in an ice-water bath, and stirred for 3 hours. Then, 8.2 parts of 3-amino-6-bromo-1,2,4-triazine were added thereto, and the reaction was continued with stirring for 6 hours. After removing the excess solvent by rotary evaporation, the product was washed with deionized water at a temperature of 2-4°C, and vacuum dried to constant weight to obtain an aminobenzophenone compound;

[0055] S12. Disperse 10 parts of an aminobenzophenone compound in acetone by weight, ultrasonically disperse for 60 min, add 1.1 parts of cyanamide, protect under nitrogen atmosphere, heat to 55-56 ° C, reflux for 36 h, and remove excess solvent by rotary evaporation to obtain a guanidinobenzophenone compound;

[0056] S13. Disperse 10 parts of 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine in DMF by weight, protect under nitrogen atmosphere, stir and mix for 30 minutes, add 0.15 parts of 1-ethyl-(3-dimethylaminopropyl)carbodiimide, continue to mix for 3 minutes, add 8.5 parts of guanidine dibenzophenone compound, heat to 115°C, stir and react for 8 hours, and then remove excess solvent by rotary evaporation to obtain an antibacterial and anti-ultraviolet intermediate;

[0057] S14. By weight, 11 parts of the antibacterial and anti-ultraviolet intermediate were mixed with 21 parts of terephthalic acid, 12 parts of ethylene glycol and 0.005 parts of butyl titanate were added, and after esterification for 4 hours, 0.002 trimethyl phosphate was added thereto, and the esterification reaction was continued for 3 hours, and then the heating was stopped and the product was extruded and cooled with cold water, and then pelletized to obtain an antibacterial and anti-ultraviolet masterbatch;

[0058] During the esterification reaction, the reaction temperature was 245°C and the reaction pressure was 0.3MPa;

[0059] S2. Mix 10 parts of PET masterbatch with 3 parts of antibacterial and anti-ultraviolet masterbatch by weight, melt at high temperature, extrude and pelletize to obtain antibacterial and anti-ultraviolet polyester masterbatch.

[0060] Embodiment 5. A method for preparing an antibacterial and anti-ultraviolet polyester masterbatch, comprising the following steps:

[0061] Compared with Example 4, this example increases the amount of the guanidinobenzophenone compound added in step S13;

[0062] S1. Preparation of antibacterial and anti-ultraviolet masterbatch;

[0063] S11. According to the weight percentage, under the protection of nitrogen atmosphere, 10 parts of 2,4-dihydroxybenzophenone were dispersed in a mixed solvent of acetone and deionized water in a volume ratio of 3:1, and after stirring evenly, 2 parts of sodium hydroxide were added thereto, and the mixture was cooled to a constant temperature in an ice-water bath, and stirred for 3 hours. Then, 8.2 parts of 3-amino-6-bromo-1,2,4-triazine were added thereto, and the reaction was continued with stirring for 6 hours. After removing the excess solvent by rotary evaporation, the product was washed with deionized water at a temperature of 2-4°C, and vacuum dried to constant weight to obtain an aminobenzophenone compound;

[0064] S12. Disperse 10 parts of an aminobenzophenone compound in acetone by weight, ultrasonically disperse for 60 min, add 1.1 parts of cyanamide, protect under nitrogen atmosphere, heat to 55-56 ° C, reflux for 36 h, and remove excess solvent by rotary evaporation to obtain a guanidinobenzophenone compound;

[0065] S13. Disperse 10 parts of 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine in DMF by weight, protect under nitrogen atmosphere, stir and mix for 30 minutes, add 0.15 parts of 1-ethyl-(3-dimethylaminopropyl)carbodiimide, continue to mix for 3 minutes, add 10.2 parts of guanidine dibenzophenone compound, heat to 115°C, stir and react for 8 hours, and then remove excess solvent by rotary evaporation to obtain an antibacterial and anti-ultraviolet intermediate;

[0066] S14. By weight, 11 parts of the antibacterial and anti-ultraviolet intermediate were mixed with 21 parts of terephthalic acid, 12 parts of ethylene glycol and 0.005 parts of butyl titanate were added, and after esterification for 4 hours, 0.002 trimethyl phosphate was added thereto, and the esterification reaction was continued for 3 hours, and then the heating was stopped and the product was extruded and cooled with cold water, and then pelletized to obtain an antibacterial and anti-ultraviolet masterbatch;

[0067] During the esterification reaction, the reaction temperature was 245°C and the reaction pressure was 0.3MPa;

[0068] S2. Mix 10 parts of PET masterbatch with 3 parts of antibacterial and anti-ultraviolet masterbatch by weight, melt at high temperature, extrude and pelletize to obtain antibacterial and anti-ultraviolet polyester masterbatch.

[0069] Embodiment 6. A method for preparing an antibacterial and anti-ultraviolet polyester masterbatch, comprising the following steps:

[0070] Compared with Example 5, this embodiment increases the amount of antibacterial and anti-ultraviolet intermediate added in step S14;

[0071] S1. Preparation of antibacterial and anti-ultraviolet masterbatch;

[0072] S11. According to the weight percentage, under the protection of nitrogen atmosphere, 10 parts of 2,4-dihydroxybenzophenone were dispersed in a mixed solvent of acetone and deionized water in a volume ratio of 3:1, and after stirring evenly, 2 parts of sodium hydroxide were added thereto, and the mixture was cooled to a constant temperature in an ice-water bath, and stirred for 3 hours. Then, 8.2 parts of 3-amino-6-bromo-1,2,4-triazine were added thereto, and the reaction was continued with stirring for 6 hours. After removing the excess solvent by rotary evaporation, the product was washed with deionized water at a temperature of 2-4°C, and vacuum dried to constant weight to obtain an aminobenzophenone compound;

[0073] S12. Disperse 10 parts of an aminobenzophenone compound in acetone by weight, ultrasonically disperse for 60 min, add 1.1 parts of cyanamide, protect under nitrogen atmosphere, heat to 55-56 ° C, reflux for 36 h, and remove excess solvent by rotary evaporation to obtain a guanidinobenzophenone compound;

[0074] S13. Disperse 10 parts of 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine in DMF by weight, protect under nitrogen atmosphere, stir and mix for 30 minutes, add 0.15 parts of 1-ethyl-(3-dimethylaminopropyl)carbodiimide, continue to mix for 3 minutes, add 10.2 parts of guanidine dibenzophenone compound, heat to 115°C, stir and react for 8 hours, and then remove excess solvent by rotary evaporation to obtain an antibacterial and anti-ultraviolet intermediate;

[0075] S14. By weight, 18 parts of the antibacterial and anti-ultraviolet intermediate were mixed with 21 parts of terephthalic acid, 12 parts of ethylene glycol and 0.005 parts of butyl titanate were added, and after esterification for 4 hours, 0.002 trimethyl phosphate was added thereto, and the esterification reaction was continued for 3 hours, and then the heating was stopped and the product was extruded and cooled with cold water, and then pelletized to obtain an antibacterial and anti-ultraviolet masterbatch;

[0076] During the esterification reaction, the reaction temperature was 245°C and the reaction pressure was 0.3MPa;

[0077] S2. Mix 10 parts of PET masterbatch with 3 parts of antibacterial and anti-ultraviolet masterbatch by weight, melt at high temperature, extrude and pelletize to obtain antibacterial and anti-ultraviolet polyester masterbatch.

[0078] Comparative Example 1. A method for preparing an antibacterial and anti-ultraviolet polyester masterbatch, comprising the following steps:

[0079] Compared with Example 1, this comparative example did not prepare an antibacterial and anti-ultraviolet intermediate;

[0080] S1. By weight, 21 parts of terephthalic acid, 12 parts of ethylene glycol and 0.005 parts of butyl titanate were mixed, and after esterification for 4 hours, 0.002 trimethyl phosphate was added thereto, and the esterification reaction was continued for 3 hours, and the heating was stopped and the product was extruded and cooled with cold water, and pelletized to obtain an antibacterial and anti-ultraviolet masterbatch;

[0081] During the esterification reaction, the reaction temperature was 245°C and the reaction pressure was 0.3MPa;

[0082] S2. Mix 10 parts of PET masterbatch with 3 parts of antibacterial and anti-ultraviolet masterbatch by weight, melt at high temperature, extrude and pelletize to obtain antibacterial and anti-ultraviolet polyester masterbatch.

[0083] Testing: The polyester masterbatches prepared in Examples 1-6 and Comparative Example 1 were processed into test specimens;

[0084] According to GB / T 20944.3-2008, the test strips prepared in Examples 1-6 and Comparative Example 1 were tested for antibacterial and antimicrobial properties against Staphylococcus aureus, Escherichia coli, and Candida albicans;

[0085] According to GB / T 1040.2-2022, the tensile strength and elongation at break of the test specimens prepared in Examples 1-6 and Comparative Example 1 were tested;

[0086] According to GB / T 16422.2-2022, the test specimens prepared in Examples 1-6 and Comparative Example 1 were aged. The aging equipment used a xenon arc lamp and a daylight filter to simulate sunlight irradiation. The aging cycle conditions were 102 minutes of illumination, followed by 18 minutes of illumination and spraying. The wavelength of the light was 340 nm and the power was 0.51 W / (m 2 ·nm), the test chamber temperature is 35±2℃, the relative humidity is 60±5%, and after 120h of aging test, the tensile strength and elongation at break are tested again;

[0087] The test results are shown in the table below;

[0088]

[0089] Finally, it should be noted that the above description 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 an antibacterial and anti-ultraviolet polyester masterbatch, characterized in that: The following steps are involved: S1. Preparation of antibacterial and anti-ultraviolet masterbatch; S11. Under nitrogen atmosphere protection, 2,4-dihydroxybenzophenone was dispersed in a mixed solvent of acetone and deionized water in a volume ratio of 3:1, and after stirring evenly, sodium hydroxide was added thereto, and the mixture was cooled to a constant temperature in an ice-water bath, and stirred for 2-4 hours, and 3-amino-6-bromo-1,2,4-triazine was added thereto, and the reaction was continued with stirring for 4-8 hours. After removing the excess solvent by rotary evaporation, the product was washed with deionized water at a temperature of 0-5°C, and vacuum dried to constant weight to obtain an aminobenzophenone compound; S12. The aminobenzophenone compound is dispersed in acetone, ultrasonically dispersed for 40-80 min, and then cyanamide is added thereto, and the mixture is protected by a nitrogen atmosphere, and the temperature is raised to 55-56° C., and the mixture is refluxed for 12-48 h, and then the excess solvent is removed by rotary evaporation to obtain a guanidinobenzophenone compound; S13. Disperse 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine in DMF, protect under nitrogen atmosphere, stir and mix for 15-45 minutes, add 1-ethyl-(3-dimethylaminopropyl)carbodiimide, continue to mix for 3-5 minutes, add guanidinobenzophenone compound, heat to 115-120° C., stir and react for 4-12 hours, and remove excess solvent by rotary evaporation to obtain an antibacterial and anti-ultraviolet intermediate; S14. The antibacterial and anti-ultraviolet intermediate is mixed with terephthalic acid, ethylene glycol and butyl titanate are added, and the esterification reaction is continued for 3-5 hours, and trimethyl phosphate is added thereto. After the esterification reaction is continued for 2-4 hours, the heating is stopped and the product is extruded and cooled with cold water, and then pelletized to obtain an antibacterial and anti-ultraviolet masterbatch; S2. Mix the PET masterbatch and the antibacterial and anti-ultraviolet masterbatch by weight, melt them at high temperature, extrude and pelletize them to obtain the antibacterial and anti-ultraviolet polyester masterbatch.

2. The method for preparing an antibacterial and anti-ultraviolet polyester masterbatch according to claim 1, characterized in that: In terms of weight, in step S11, the mass ratio of 2,4-dihydroxybenzophenone, sodium hydroxide and 3-amino-6-bromo-1,2,4-triazine is 10:(1.5-2):(6-8.2).

3. The method for preparing an antibacterial and anti-ultraviolet polyester masterbatch according to claim 1, characterized in that: In terms of parts by weight, in step S12, the mass ratio of the aminobenzophenone compound to cyanamide is 10:(0.9-1.1).

4. The method for preparing an antibacterial and anti-ultraviolet polyester masterbatch according to claim 1, characterized in that: In terms of weight, in step S13, the mass ratio of the 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine, 1-ethyl-(3-dimethylaminopropyl)carbodiimide, and guanidinobenzophenone compound is 10:(0.15-0.2):(8.5-10.2).

5. The method for preparing an antibacterial and anti-ultraviolet polyester masterbatch according to claim 1, characterized in that: In terms of weight, in step S14, the mass ratio of the antibacterial and anti-ultraviolet intermediate, terephthalic acid, and ethylene glycol is (11-18): (20-24):

12.

6. The method for preparing an antibacterial and anti-ultraviolet polyester masterbatch according to claim 1, characterized in that: In terms of weight, in step S14, the mass ratio of the antibacterial and anti-ultraviolet intermediate, butyl titanate, and trimethyl phosphate is (11-18): (0.005-0.01): (0.002-0.005).

7. The method for preparing an antibacterial and anti-ultraviolet polyester masterbatch according to claim 1, characterized in that: In step S14, the esterification reaction temperature is 240-260° C., and the esterification reaction pressure is 0.1-4 MPa.

8. The method for preparing an antibacterial and anti-ultraviolet polyester masterbatch according to claim 1, characterized in that: In terms of weight, in step S2, the mass ratio of the PET masterbatch to the antibacterial and anti-ultraviolet masterbatch is 10:(3-5).

9. An antibacterial and anti-ultraviolet polyester masterbatch prepared by the preparation method according to any one of claims 1 to 8.

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