Preparation and application of antibacterial masterbatch for polyester fiber

Preparation and application of antibacterial masterbatch for polyester fiber

Abstract : An antibacterial plastic masterbatch specially designed for the preparation of antibacterial synthetic fibers is introduced , which uses a silver-containing co-contained composition with a high melt index.

The polymer resin is kneaded , and then blended with a carrier resin , melt-extruded and pelletized by a twin-screw extruder. The masterbatch and the PET resin were mixed to prepare a polyester fiber with good antibacterial properties.

Antibacterial materials, the silver-based antibacterial agent is not decomposed because of persistent, broad spectrum antibiotic resistant bacteria easily induced, antibacterial ability, high safety performance, plastic or the like prepared to a suitable antimicrobial article [1-2].

At present, most of the silver-containing antibacterial polymer materials adopt the carrier introduction method , which belongs to the "macro-fake compatibility method". In general, the downloaded body is an inorganic powder , and the nano-loaded silver inorganic powder itself has hard agglomeration and is poorly compatible with the polymer material and is difficult to disperse [3] . The fiber drawing causes adverse effects such as poor continuity, low breaking strength, and reduced aging resistance.

On the other hand , in the inorganic powder , most of the silver ions are fixed or encapsulated by the inorganic lattice , and are not easily released. At the same time , the calcination process will cause the surface silver ions to change into a zero valence state [4] . These factors can lead to a decline in antibacterial ability , so it is necessary to introduce

Excess silver is added to compensate for the decline in antibacterial capacity , thus causing waste.

Another method of adding silver is prepared using elemental nanosilver antibacterial plastic masterbatch. At present, the nano silver used is mostly prepared by an aqueous solution reduction method , and then subjected to concentration, dehydration, etc. , and finally blended with the resin. The nano-silver element added by this post-mixing method has no compatibility with the resin , and it is necessary to introduce a compatibilizer or a dispersant. In actual use, it is often not fully dispersed , resulting in agglomeration beyond the nanoscale. Therefore , the nano-silver element added by this post-mixing method is not very satisfactory for the fiber product. To this end , this paper explores the new silver-containing antibacterial masterbatch for polyester fiber products.

2 micro homogeneous dispersion of silver prepared antimicrobial masterbatch

2. 1 Preparation of silver-containing co-content composition

The silver-containing co-compound composition is composed of a silver salt, a dispersant, a bulking agent, a graft modifier, a shaping resin, and the like. It is formed by kneading at 170 to 200 °C. Then cooled, discharged , and crushed by a plastic crusher. 5mm The following powders are reserved. The shaping resin is made of PET .

2. Preparation of 2 silver-containing antibacterial masterbatch

The co-contained composition is mixed with PET , melt co-extruded by a co-rotating twin-screw extruder , water-cooled , pelletized , dried , and packaged to obtain a PET antibacterial masterbatch. Twin-screw extruder : Model TE-34, Nanjing Keya Company , main engine current : 14 ~ 17 A; main engine speed : 800 ~ 1 000r / min; feeding speed : 600 ~ 700 r / min; pelletizer speed : 1 000 to 1 100 r /min . Where the PET fiber grade polyester chips using 18 southeast of Yizheng Chemical Fiber & Textile Technology a Chemical Fiber & Textile Technology WB 2009 Nian 3 Yue chemical fiber raw materials Co., Ltd. - 8828B. The temperature control of each zone in 1 to 8 zones is : 235 °C , 255 °C , 270 °C , 275 °C , 280 °C , 280 °C , 275 °C with 270 °C .

3 Preparation of antibacterial polyester fiber

The antibacterial Masterbatch PET 1%, 2% ratio PET material added WB - 8828B, a uniformly mixed in a mixer, and then added to a spinning machine drawing. Process : batching→mixing→drum drying→spinning→winding→dropping→bundling→stretching→tension heat setting→curling→relaxing heat setting→cutting→packing. Main spinning and post-processing conditions : spinning speed 1 200m /min, melt temperature 275 °C , FR - 1 speed 1 600 r / min, FR - 2 speed 1 600 r / min, SR speed 1 900 r / min, DF - 3 vapor pressure of 1. 0 ~ 1. 2MPa, HF vapor pressure of 1. 2MPa, total Drawing ratio 4. 03 .

4 analysis and performance testing [5]

4. 1 toxicological experiment of antibacterial masterbatch

Refer to the Ministry of Health of the People's Republic of China 2002 "Disinfection Technical Specifications" (2002 Edition ) Part II 2. 3. 1 ( Acute oral toxicity test ), the test results were provided by Guangdong Provincial Health Inspection Center.

4. 2 antibacterial properties of antibacterial fiber

Fiber antibacterial performance test refers to GB / T 20944 "Evaluation of antibacterial properties of textiles" Part 2 : Absorption method. The test data was provided by the Guangdong Provincial Microbial Analysis and Testing Center.

4. 3 fiber toxicology test

Refer to the Ministry of Health of the People's Republic of China 2002 "Disinfection Technical Specifications" (2002 Edition ) Part II 2. 3. 3 ( skin irritation test ), 2. 3. 5 ( Vaginal mucosal irritation test ), 2. 3. 6 ( skin allergy test ) . The test results were provided by the Shanghai Institute of Preventive Medicine.

4. 4 fiber mechanical properties test

Referring to the relevant standards, testing by the Shenzhen Polytechnic.

5 results and discussion

5. 1 formula design

In order to solve the problem of particle agglomeration , a silver co-compound composition is employed. In this form of combination thereof silver are: ionic form, molecular form, and a small amount of nano silver in the form of a simple substance and binding polymer. The dispersion of silver is at the molecular level , which is a microscopic uniform state , and there is no agglomerated particles. Considering the dispersion stability of the silver composition, and the feasibility of processing requirements, for the polyester masterbatch PET employed high melt index as a carrier. Figure 1 , Figure 2 , and Figure 3 show the comparison of the antibacterial masterbatch with the other two different antibacterial masterbatch on the market under the microscope (200 times ) .

Contrast the above three sections masterbatch microscope image can be seen, there are no particles present antimicrobial masterbatch is present, it is an overall homogeneous structure. Particulate matter can be clearly seen in the masterbatch containing the inorganic antibacterial powder. In the image of the master particle slice containing the nano-silver element , it can be seen that the nano-silver particles are too large to form a black particle accumulation region , and the distribution is uneven. According to the present antibacterial masterbatch production antibacterial fiber during drawing, and no clogging of the screen orifices phenomena no yarn.

5. 2 toxicological test of antibacterial masterbatch

Weigh the antibacterial masterbatch ( containing 0.5% of silver ) 11g , 4% glacial acetic acid 50mL, sealed in a container after 72h immersion filtration, acetic acid until complete evaporation, the residue was distilled water as solvent is the test volume to 20mL thereof. 0. 2mL / 20g Gavage needle body weight fed a test substance to N IH mice were poisoning, the number of deaths and the time of death were observed twice daily for 2 weeks observation period. The acute oral toxicity test of the test substance on N IH mice is shown in Table 1 . Found: observation period, the subject N IH no obvious symptoms of mice, no deaths occurred. Therefore , the acute oral LD50 of the antibacterial masterbatch for N IH mice is > 5 000 mg/kg, which is an actual non-toxic grade. 19, No. 1 Fiber & Textile Technology in March 2009 Chemical Fiber & Textile Technology Table mg · kg- 1 1 Number of test substance toxicity gender NIH mice acute oral dose / animal / bird deaths / mortality only,% Female 5 500 10 0 0 male 5 500 10 0 0

5. 3 antibacterial properties of antibacterial polyester fiber

Due to the high temperature during processing , some of the silver ions are reduced to nano-silver , and the fiber exhibits a golden yellow color unique to nano-silver , which is more uniform and less granular than the previously mixed nano-silver. The experiment also tested the photochromism of the 2% antibacterial masterbatch polyester fiber , which was left in the sun for 15 days and its color was unchanged. The test results of the antibacterial properties of the products are shown in Table 2 . Table 2 : bactericidal effect of antibacterial polyester fiber sterilization effect , % masterbatch addition amount 1. 0%, product silver content 5 × 10- 5 masterbatch addition amount 2. 0%, product silver content 1 × 10- 4 golden yellow Staphylococcus ATCC 653899. 23 99. 87 Escherichia coli ATCC 2592299. 54 99. 91 Candida albicans ATCC 1023199. 10 99. 75 Note : The number of control bacteria of Escherichia coli, Staphylococcus aureus and Candida albicans is 1. 8 × 105 cfu /mL , 1. 5 × 105 cfu /mL , 1. 3 × 105cfu /mL . It can be seen from Table 2 that a good antibacterial effect can be achieved by adding 1% to 2% of the product using the antibacterial masterbatch.

5. 4 Toxicological test of antibacterial polyester fiber

Antibacterial fiber is in contact with the human body , and its safety performance should be placed first. We studied the toxicological testing of these antimicrobial article, wherein the skin irritation test, vaginal mucous membrane irritation test, the skin allergy test animals used were New Zealand rabbits normal level, normal SD rats and the general level Albino Guinea British species, The test results are shown in Table 3 . As can be seen from Table 3 , the antibacterial polyester fiber has no irritation to the skin and vaginal mucosa , and the sensitizing strength is extremely light , showing a high degree of safety. Table 3 Toxicological test results of antibacterial fiber Test sample Toxicological test item Skin irritation Vaginal mucosa irritation Skin allergic reaction Antibacterial polyester fiber Non-irritating, non-irritating Sensitizing intensity is extremely light Note : It is made with a product with 2% antibacterial masterbatch Test sample

5. 5 mechanical properties test of antibacterial polyester fiber [6]

The prepared antibacterial polyester fiber is 75dtex/ 24f The mechanical properties test results are shown in Table 4 . Table 4 Mechanical properties of antibacterial polyester fiber Fiber breaking strength / cN · dtex - 1 Young's modulus / cN · dtex - 1 elongation at break , % without antibacterial masterbatch 3. 96 1. 22 11. 23 plus 1% Antibacterial masterbatch 3. 91 1. 26 11. 98 plus 2% antibacterial masterbatch 3. 76 1. 31 12. 85 From the test results of the mechanical properties of the antibacterial polyester fiber of Table 4 , compared with the pure polyester fiber sample , antibacterial masterbatch added little effect on the fracture strength of the polyester fiber and the mechanical properties of Young's modulus, elongation at break with increasing addition of base particles is increased, the impact of which the low molecular weight graft resin base particles and a solvent relevant .

6 conclusion

In this paper, a PET composition is extruded molten resin in the production of a specific antimicrobial polyester fiber antibacterial plastic masterbatch was prepared containing a total silver content, the results obtained by studying the following: (1) a polyester prepared with nontoxic antimicrobial masterbatch genus substance. (2) When the amount of antibacterial masterbatch is between 1% and 2% , the polyester fiber has good antibacterial properties and is advantageous for cost reduction. (3) antibacterial polyester fibers prepared from the masterbatch of a golden yellow antimicrobial and exhibits good light stability. (4) The polyester fiber prepared from the antibacterial masterbatch has no irritation to the skin and vaginal mucosa , and the sensitization intensity is extremely light , and other performance indexes are in line with national standards.

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