CN109135208A - A kind of PET antibacterial matrices and preparation method thereof - Google Patents
A kind of PET antibacterial matrices and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of PET antibacterial matrices and preparation method thereof.The PET antibacterial matrices are prepared by the raw material of following mass parts: 70-100 parts of PET resin, 1-8 parts of metal antibacterial agent, 5-10 parts of fire retardant, is modified sisal fiber 10-25 parts, 0.1-0.5 parts of coupling agent at 1-5 parts of dispersing agent.Preparation process of the present invention is simple, easily operated, and the PET antibacterial matrices prepared and polyester plastics are compound with good dispersibility and compatibility, shows excellent antibacterial ability, flame retardant property and mechanical property, there is wide application prospect.
Description
Technical field
The present invention relates to technical field of polymer materials, and in particular to a kind of PET antibacterial matrices and preparation method thereof.
Background technique
With the development and the improvement of people's living standards of social economy, the application field of plastic products is also constantly expanding
Greatly, small common into life various shopping bags, refuse bag, plastic barrel and packaging bag etc., arrive greatly automobile, household electrical appliances, communication, height
The industries such as shelves tool, the application field of plastic products are also slowly developing to advanced industry field while constantly widening, phase
For common application industry, the quality requirements in advanced field are higher, it is desirable to which plastic products have better quality.Wherein PET is (poly-
Ethylene glycol terephthalate) because having excellent heat resistance, corrosion-resistant, obdurability, electrical insulating property etc., and it is cheap, and
It is used widely in plastic applications such as fiber, film, engineering plastics.PET is a kind of crystallization linear polyesters, has good gas
Body barrier property, toughness, extensibility and mechanical strength, and there is the excellent transparency and environment friendly, but unmodified PET is certainly
Body flame retardant property is inadequate, to limit its application in every field.
In order to improve the performance of plastic products, common method is that filler parent granule is added to be modified.Current Domestic
How the external field is mainly around improving dispersibility, thin-film transparent, interface interaction, power of the filler in plastic substrate
The comprehensive performances such as performance, hardness performance, absorptivity, shock resistance are learned to be unfolded.By inorganic filler (such as calcium carbonate, talcum
Powder, kaolin, wollastonite etc.) suitably it is surface-treated, vector resin and dispersing agent are added, is penetrated into plastic substrate, is made
It is standby at filler parent granule eventually in plastic products.Currently, in the filling-modified research of plastics and its product, calcium carbonate applications
Most commonly used inorganic filler, but its oil factor is big, product light absorptive is high, sub- face and atomized surface effect can be presented in product surface, and
Loading, which crosses conference, makes the mechanical property degradation of product, tends not to meet high tenacity, high strength, high tenacity product
Demand.
Therefore, a kind of PET antibacterial matrices are developed to have practical significance.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, the present invention provides a kind of PET antibacterial matrices and preparation method thereof.
A kind of PET antibacterial matrices, raw material include: 70-100 parts of PET resin, 1-5 parts of dispersing agent, metal in parts by mass
1-8 parts of antibacterial agent, 5-10 parts of fire retardant, sisal fiber or sisal fiber 10-25 parts, 0.1-0.5 parts of coupling agent modified.
Preferably, the PET antibacterial matrices are prepared by the raw material of following mass parts: 70-100 parts of PET resin, dispersion
1-5 parts of agent, 5-10 parts of fire retardant, is modified sisal fiber 10-25 parts, 0.1-0.5 parts of coupling agent at 1-8 parts of metal antibacterial agent.
The dispersing agent includes one of zinc stearate, polyethylene wax, calcium stearate or a variety of.
The fire retardant includes one of diethyl zinc hypophosphite, melamine phosphate, composite flame-retardant agent or a variety of.
Preferably, the fire retardant by diethyl zinc hypophosphite, melamine phosphate, composite flame-retardant agent in mass ratio
(1-6): (1-6): (1-6) is mixed.
The coupling agent includes hexamethyldisilazane, dimethoxydimethylsilane, phenyl triethoxysilane, γ-
One of mercaptopropyltriethoxysilane is a variety of.
The metal antibacterial agent the preparation method comprises the following steps: weigh 5-10 parts of copper, 2-4 parts of zinc, 6-9 parts of silver by mass parts, mix
After obtain mixed-powder；Dehydrated alcohol, N- aminoethyl-γ-aminopropyltrimethoxysilane, institute are added into gained mixed-powder
Stating mixed-powder, dehydrated alcohol, N- aminoethyl-γ-aminopropyltrimethoxysilane mass ratio is 1:(1-3): (0.05-
0.1) mixture is obtained after, being mixed, gained mixture carries out ultrasonic disperse processing under the protection of argon gas, up to metal after drying
Antibacterial agent.
The composite flame-retardant agent is prepared from the following materials by weight percent: triammonium phosphate 18-30%, barium metaborate
1-4%, magnesium hydroxide 6-12%, calcium oxide 1-3%, dipentaerythritol 8-15%, modifying agent 0.5-1.5%, surplus are poly- phosphorus
Sour ammonium.
The composite flame-retardant agent the preparation method comprises the following steps: by weight percent ratio weigh each raw material component；First by tricresyl phosphate
Ammonium, ammonium polyphosphate mixing, modifying agent is added after mixing, is placed at 50-95 DEG C and is stirred, added after mixing barium metaborate,
Magnesium hydroxide, calcium oxide, dipentaerythritol, after mixing to obtain the final product.
The modified sisal fiber is the preparation method comprises the following steps: sisal fiber is added molten to the ammonium hydroxide that concentration is 0.1-0.3mol/L
In liquid, wherein the mass volume ratio of the sisal fiber and ammonia spirit is 1:(1-5) (g/mL), mixed after ultrasonic treatment
Object；It is subsequently added into the plant extracts of mixture quality 1-3%, continues to be ultrasonically treated, filtered fibre is obtained after filtering
Dimension, washs filtered fiber with water, washing to neutrality, and modified sisal fiber is obtained after dry.
The plant extracts includes one of mint extract, bajiao banana leaf extract, Eucalyptus extract or a variety of.
Preferably, the plant extracts is by mint extract, bajiao banana leaf extract, Eucalyptus extract (1- in mass ratio
6): (1-6): (1-6) is mixed.
The preparation method of the PET antibacterial matrices, comprising the following steps:
I, weighs each raw material component by mass parts composition, obtains mixture after mixing；
Above-mentioned mixture feeding double screw extruder is granulated by II, obtains PET antibacterial matrices after cooling, drying.
By adopting the above-described technical solution, compared with prior art, the present invention has the following advantages: system of the present invention
Standby simple process, easily operated, the PET antibacterial matrices prepared are compound with good dispersibility and compatible with polyester plastics
Property, excellent antibacterial ability, flame retardant property and mechanical property are shown, and environmental pollution is smaller, there is broader answer
Use prospect.
Specific embodiment
Foregoing invention content of the invention is described in further detail With reference to embodiment, but should not be incited somebody to action
This range for being interpreted as the above-mentioned theme of the present invention is only limitted to following embodiments.
Each raw material and equipment introduction in embodiment:
PET resin, model PTX142, density 1.26g/cm3, it is purchased from DuPont Corporation.
Zinc stearate, No. CAS: 557-05-1,200 mesh, product number: 1227155670, purchased from the purple chemical reagent work in Shanghai.
Copper, powdered, 100 mesh of partial size, product number HT-2 lead to powder new material Co., Ltd purchased from Luohe City China.
Zinc, powdered, 100 mesh of partial size, article No. 0010 create dew Materials Co., Ltd purchased from Hunan.
Silver, powdered, 100 mesh of partial size, model AGN-A15HZ50 are purchased from Suzhou Pu Yuandi new material Co., Ltd.
N- aminoethyl-γ-aminopropyltrimethoxysilane, No. CAS: 1760-24-3, product number: N818618 is purchased from
Shanghai Mike's woods biochemical technology Co., Ltd.
The metal antibacterial agent the preparation method comprises the following steps: according to mass parts weigh 8 parts of copper, 2 parts of zinc, silver 6 parts, obtained after mixing
Mixed-powder；Dehydrated alcohol, N- aminoethyl-γ-aminopropyltrimethoxysilane, the mixing are added into gained mixed-powder
Powder, dehydrated alcohol, N- aminoethyl-γ-aminopropyltrimethoxysilane mass ratio be 1:1.5:0.05, at 30 DEG C with
After the revolving speed stirring 30min of 68r/min, mixture is obtained, gained mixture ultrasonic disperse 30min under the protection of argon gas,
Described in the supersonic frequency of ultrasonic disperse be 28kHz, ultrasonic power 600W, dry 5h is at 60 DEG C to get metal antibacterial agent.
Diethyl zinc hypophosphite, No. CAS: 284685-45-6, average grain diameter is less than 40 μm, model FR-ZDP, is purchased from Guangzhou
Yin Yuan new material Science and Technology Ltd. of city.
Melamine phosphate, No. CAS: 20208-95-1, product number: M850103 is purchased from Shanghai Mike woods biochemistry section
Skill Co., Ltd
Triammonium phosphate, No. CAS: 10124-31-9, it is purchased from Shanghai Peng Suo biochemical technology Co., Ltd.
Barium metaborate, No. CAS: 13701-59-2,325 mesh of granularity is purchased from Zhengzhou City Zhongyuan District Yuan Feng chemical products firm.
Magnesium hydroxide, No. CAS: 1309-42-8,325 mesh of granularity is purchased from Guangzhou Ze Dan deer trade Co., Ltd.
Calcium oxide, No. CAS: 73018-51-6,125 mesh of granularity is purchased from Shenzhen Lv Li Science and Technology Ltd..
Dipentaerythritol, No. CAS: 126-58-9, product number: D806414, it is limited purchased from Shanghai Mike woods biochemical technology
Company.
Stearic acid, No. CAS: 57-11-4, product number: S108289, it is limited purchased from Shanghai Aladdin biochemical technology share
Company.
Ammonium polyphosphate, No. CAS: 14728-39-3, average degree of polymerization is greater than 200, model APP II, is purchased from Jinan person of outstanding talent nation
Work Co., Ltd.
Gamma-aminopropyl-triethoxy-silane, No. CAS: 919-30-2, product number: A10668, purchased from AlfaAesar (in
State) Chemical Co., Ltd..
Dried peppermint leaf, kind American mint, article No. bcxm041 are provided by hundred hay-scented fragrant plant Co., Ltd of Qingdao.
Leaf of Japanese banana, bajiao banana kind are Saigon any of several broadleaf plants, place of production Nanning.
Eucalyptus, kind Eucalyptus urophylla-grandis, wood chip shape are provided by Nan Jing of Zhangzhou City of Fujian Province state-owned forest farms.
Sisal fiber, specification 90mm, primes are purchased from Longzhou strength Ma Ye Co., Ltd.In the embodiment of the present invention
Before using sisal fiber, the staple fiber of 3mm long is first cut short into.
Mint extract the preparation method comprises the following steps: dried peppermint leaf is taken to be placed at 55 DEG C dry 48h, be crushed to 80 mesh, obtain peppermint
Powder；Above-mentioned peppermint powder is placed in 2L extraction tank, 4 times of peppermint powder quality of 50wt% ethanol water is added, it is super to face
Boundary extracts 2.5h, extracting pressure 20MPa, and 40 DEG C of extraction temperature, separating pressure 5MPa, obtains overcritical extraction by 35 DEG C of separation temperature
Take object and super critical extract remainder；20 times of super critical extract remainder quality of 50wt% methanol-water is added into above-mentioned super critical extract remainder
Solution is placed at 60 DEG C and is ultrasonically treated 20min, and the ultrasonic power of the ultrasonic treatment is 350W, supersonic frequency 30kHz, obtains
To ultrasonic extraction liquid；Merge above-mentioned supercritical extract and ultrasonic extraction liquid, through 150 mesh filter-cloth filterings, gained filtrate is placed in 50
DEG C, water content is concentrated under conditions of being 0.05MPa is 4% to absolute pressure, obtain mint extract.
Bajiao banana leaf extract the preparation method comprises the following steps: leaf of Japanese banana is cleaned, remove soil and sundries, be cut into the left side 5cm × 5cm
Right fragment, then the dry 12h at 80 DEG C, is crushed to 40 mesh, obtains dry powder；The hydrogen-oxygen of 10w% is added into gained dry powder
Change sodium water solution, wherein the mass volume ratio of the dry powder and sodium hydrate aqueous solution is 1:3 (g/mL), is extracted at 80 DEG C
45min, through 80 mesh filter-cloth filterings, gained filtrate is placed in 50 DEG C, absolute pressure is concentrated into water content under conditions of being 0.08MPa and is
4%, obtain the bajiao banana leaf extract.
The preparation method of Eucalyptus extract is identical as the preparation method of bajiao banana leaf extract.
Ultrasonic disperse processing equipment is VGT-1012F type nano-dispersed instrument, limited purchased from the solid special washing/cleaning equipment of Shenzhen's prestige
Company.
Supercritical extracting equipment is HY-OES-2L type supercritical extractor, limited purchased from Dongguan City ocean ultrasonic wave science and technology
Company.
Ultrasound processing equipment is VS-040HAL type high-frequency ultrasonic cleaning machine, purchased from the fertile letter limited public affairs of instrument manufacturing in Wuxi
Department.
Milling apparatus is JMF-80 type rubber mill, is purchased from Guangzhou Heng Dong mechanical equipment Science and Technology Ltd..
Embodiment 1
A kind of PET antibacterial matrices, are prepared by the raw material of following mass parts: 90 parts of PET resin, 3 parts of zinc stearate, gold
Belong to 5 parts of antibacterial agent, 2 parts of diethyl zinc hypophosphite, 2 parts of melamine phosphate, 2 parts of composite flame-retardant agent, 10 parts of sisal fiber,
0.3 part of gamma-mercaptopropyltriethoxysilane.
Composite flame-retardant agent the preparation method comprises the following steps: by weight percent ratio weigh triammonium phosphate 20%, barium metaborate 3%,
Magnesium hydroxide 8%, calcium oxide 1%, dipentaerythritol 8%, stearic acid 1%, ammonium polyphosphate 59%；First by triammonium phosphate, poly- phosphorus
The mixing of sour ammonium is first placed in 30 DEG C, stirs 20min under conditions of 500r/min, stearic acid is subsequently added into, in 50 DEG C, 1000r/min
Under conditions of stir 5min, add barium metaborate, magnesium hydroxide, calcium oxide, dipentaerythritol, continue in 30 DEG C, 500r/
Under conditions of min stir 40min to get.
The preparation method of the PET antibacterial matrices, comprising the following steps:
I, weighs and mixes each raw material component by mass parts composition, stirs 20min under conditions of 300r/min, 40 DEG C,
Obtain mixture；
Above-mentioned mixture feeding double screw extruder is granulated by II, and nine temperature are wherein divided into double screw extruder
Area is spent, area's temperature is 190 DEG C, and two area's temperature are 200 DEG C, and three area's temperature are 240 DEG C, and four area's temperature are 230 DEG C, five area's temperature
It is 230 DEG C, six area's temperature are 235 DEG C, and seven area's temperature are 235 DEG C, and eight area's temperature are 235 DEG C, and nine area's temperature are 225 DEG C, head
Temperature is 230 DEG C, and screw speed is 180r/min clock, and mixture melted by heat is passed through in the case where the screw rod of double screw extruder pushes
The outflow of poroid mouth mold, through stock-cutter earnestly at the cylindrical pellets of 3mm × 3mm after being cooled to 30 DEG C, dry 30min at 100 DEG C,
Up to PET antibacterial matrices.
Embodiment 2
Substantially the same manner as Example 1, difference is only in that:
The PET antibacterial matrices are prepared by the raw material of following mass parts: 90 parts of PET resin, 3 parts of zinc stearate, gold
Belong to 5 parts of antibacterial agent, 3 parts of diethyl zinc hypophosphite, 3 parts of melamine phosphate, 10 parts of sisal fiber, γ-three ethoxy of mercapto propyl
0.3 part of base silane.
Embodiment 3
Substantially the same manner as Example 1, difference is only in that:
The PET antibacterial matrices are prepared by the raw material of following mass parts: 90 parts of PET resin, 3 parts of zinc stearate, gold
Belong to 5 parts of antibacterial agent, 3 parts of melamine phosphate, 3 parts of composite flame-retardant agent, 10 parts of sisal fiber, γ-mercapto propyl-triethoxysilicane
0.3 part of alkane.
Embodiment 4
Substantially the same manner as Example 1, difference is only in that:
The PET antibacterial matrices are prepared by the raw material of following mass parts: 90 parts of PET resin, 3 parts of zinc stearate, gold
Belong to 5 parts of antibacterial agent, 3 parts of diethyl zinc hypophosphite, 3 parts of composite flame-retardant agent, 10 parts of sisal fiber, γ-mercapto propyl-triethoxysilicane
0.3 part of alkane.
Comparative example 1
Substantially the same manner as Example 1, difference is only in that:
The PET antibacterial matrices are prepared by the raw material of following mass parts: 90 parts of PET resin, 3 parts of zinc stearate, gold
Belong to 5 parts of antibacterial agent, 10 parts of sisal fiber, 0.3 part of gamma-mercaptopropyltriethoxysilane.
Embodiment 5
Substantially the same manner as Example 1, difference is only in that: the sisal fiber replaces with modified sisal fiber.
The modified sisal fiber the preparation method comprises the following steps: being added sisal fiber into the ammonia spirit of 0.3mol/L,
Described in the mass volume ratio of sisal fiber and ammonia spirit be 1:3 (g/mL), be 80kHz, ultrasonic wave function in ultrasonic frequency
Rate is ultrasonication 15min under conditions of 500W, obtains mixture, mixture quality then is added into gained mixture
1.5% plant extracts continues ultrasonication under conditions of ultrasonic frequency is 80kHz, ultrasonic power is 500W
20min obtains filtered fiber through 80 mesh filter-cloth filterings, then is washed with deionized water to filtered fiber, washing
It is placed at 80 DEG C dry 6h to neutrality, obtains modified sisal fiber.
The plant extracts is by mint extract, bajiao banana leaf extract, Eucalyptus the extract quality of 1:1:1 in mass ratio
Than mixing.
Embodiment 6
Substantially the same manner as Example 1, difference is only in that: the sisal fiber replaces with modified sisal fiber.
The modified sisal fiber the preparation method comprises the following steps: being added sisal fiber into the ammonia spirit of 0.3mol/L,
Described in the mass volume ratio of sisal fiber and ammonia spirit be 1:3 (g/mL), be 80kHz, ultrasonic wave function in ultrasonic frequency
Rate is ultrasonication 15min under conditions of 500W, obtains mixture, mixture quality then is added into gained mixture
1.5% plant extracts continues ultrasonication under conditions of ultrasonic frequency is 80kHz, ultrasonic power is 500W
20min obtains filtered fiber through 80 mesh filter-cloth filterings, then is washed with deionized water to filtered fiber, washing
It is placed at 80 DEG C dry 6h to neutrality, obtains modified sisal fiber.
The plant extracts is mixed by mint extract, the bajiao banana leaf extract mass ratio of 1:1 in mass ratio.
Embodiment 7
Substantially the same manner as Example 1, difference is only in that: the sisal fiber replaces with modified sisal fiber.
The modified sisal fiber the preparation method comprises the following steps: being added sisal fiber into the ammonia spirit of 0.3mol/L,
Described in the mass volume ratio of sisal fiber and ammonia spirit be 1:3 (g/mL), be 80kHz, ultrasonic wave function in ultrasonic frequency
Rate is ultrasonication 15min under conditions of 500W, obtains mixture, mixture quality then is added into gained mixture
1.5% plant extracts continues ultrasonication under conditions of ultrasonic frequency is 80kHz, ultrasonic power is 500W
20min obtains filtered fiber through 80 mesh filter-cloth filterings, then is washed with deionized water to filtered fiber, washing
It is placed at 80 DEG C dry 6h to neutrality, obtains modified sisal fiber.
The plant extracts is mixed by bajiao banana leaf extract, the Eucalyptus extract mass ratio of 1:1 in mass ratio.
Embodiment 8
Substantially the same manner as Example 1, difference is only in that: the sisal fiber replaces with modified sisal fiber.
The modified sisal fiber the preparation method comprises the following steps: being added sisal fiber into the ammonia spirit of 0.3mol/L,
Described in the mass volume ratio of sisal fiber and ammonia spirit be 1:3 (g/mL), be 80kHz, ultrasonic wave function in ultrasonic frequency
Rate is ultrasonication 15min under conditions of 500W, obtains mixture, mixture quality then is added into gained mixture
1.5% plant extracts continues ultrasonication under conditions of ultrasonic frequency is 80kHz, ultrasonic power is 500W
20min obtains filtered fiber through 80 mesh filter-cloth filterings, then is washed with deionized water to filtered fiber, washing
It is placed at 80 DEG C dry 6h to neutrality, obtains modified sisal fiber.
The plant extracts is mixed by mint extract, the Eucalyptus extract mass ratio of 1:1 in mass ratio.
Test case 1
Anti-microbial property test: it is provided with reference to GB21551.2-2010, to the antibiotic property of PET antibacterial matrices in embodiment 1-8
It can be carried out test.Bacterium: Escherichia coli (ATCC25922), Candida albicans (ATCC10231) is used in detection.Specific test result is shown in
Table 1.
Table 1: anti-microbial property test result table
| Group | Escherichia coli sterilizing rate/% | Candida albicans sterilizing rate/% |
| Embodiment 1 | 98.1 | 97.9 |
| Embodiment 2 | 97.6 | 97.0 |
| Embodiment 3 | 97.5 | 97.3 |
| Embodiment 4 | 97.1 | 97.2 |
| Embodiment 5 | 99.5 | 98.7 |
| Embodiment 6 | 98.2 | 98.0 |
| Embodiment 7 | 98.9 | 98.3 |
| Embodiment 8 | 98.8 | 98.5 |
By test result it is found that PET antibacterial matrices of the present invention have excellent anti-microbial property.
Test case 2
Limiting oxygen index determination: the oxygen index (OI) of PET antibacterial matrices in embodiment 1-8 and comparative example 1 is tested.
Test method: first by PET antibacterial matrices in embodiment 1-8 and comparative example 1 and common PET slice (lot number 136,
Viscosity is (0.64 ± 0.01) d L/g, is purchased from Foshan FSPG Hi-Tech. Shares Co., Ltd.) it is mixed by the mass ratio of 10:90,
Be made on injection molding machine (model AMC-350, be purchased from Shenzhen Zhong Yanshentuo Science and Technology Ltd.) using conventional method 130mm ×
The plaques of 6.5mm × 3mm, common PET slice are made same size PET print also by same method, then use
Oxygen index instrument (model HC22 type is purchased from Jiangning, Nanjing analysis instrument factory), according to plastics oxygen as defined in GBT 2406.2-2009
Index method measures oxygen index (OI), and environment temperature is controlled at 25 DEG C, and testing result is as shown in table 2.
Table 2: oxygen index (OI) test result table
| Group | Oxygen index (OI)/% |
| PET | 21 |
| Embodiment 1 | 39 |
| Embodiment 2 | 34 |
| Embodiment 3 | 30 |
| Embodiment 4 | 31 |
| Comparative example 1 | 27 |
Test result in comparison sheet it is found that in embodiment 1 fire retardant by diethyl zinc hypophosphite, melamine phosphate,
Composite flame-retardant agent composition, the oxygen index (OI) of gained PET print are apparently higher than embodiment 2-4 (diethyl zinc hypophosphite, melamine phosphorus
Any the two compounding of acid esters, composite flame-retardant agent) and comparative example 1 (unused fire retardant).
Test case 3
Mechanics Performance Testing: by embodiment 1 and being that PET antibacterial matrices made from strength 5-8 are added to PET resin (type
Number PTX142, density 1.26g/cm3, it is purchased from DuPont Corporation) in, routinely the identical PET plastic of specification is made in technique,
Wherein the master batch and the mass ratio of PET resin are 20:80, then by the regulation test tensile strength of GB/T13022-1991 and
Elongation at break, test equipment are LDX-100 type tensile testing machine (being purchased from Beijing Lan Demeike Science and Technology Development Co., Ltd.), are surveyed
Examination speed is 50mm/min.As a result as shown in table 3 below.
Table 3: mechanical experimental results table
| Group | Tensile strength/Mpa | Elongation at break/% |
| PET resin | 28.3 | 390 |
| Embodiment 1 | 32.7 | 410 |
| Embodiment 5 | 46.9 | 541 |
| Embodiment 6 | 38.8 | 475 |
| Embodiment 7 | 41.3 | 483 |
| Embodiment 8 | 40.2 | 479 |
Test result in comparison sheet is it is found that fire retardant is by mint extract, bajiao banana leaf extract, Eucalyptus in embodiment 6-8
Any two kinds of components of extract are modified sisal fiber, and the mechanical property of gained PET plastic is apparently higher than 1 (sword of embodiment
Flaxen fiber is unmodified)；Further, embodiment 5 is used and is made of mint extract, bajiao banana leaf extract, Eucalyptus extract
Plant extracts is modified sisal fiber, further improves the mechanical property of PET plastic.
The above described is only a preferred embodiment of the present invention, limitation in any form not is done to the present invention, therefore
The equivalent or simple change that all principles described according to the invention patent design are done, is included in the scope of protection of the patent of the present invention
It is interior；Those skilled in the art can make various modifications or additions to the described embodiments
Or be substituted in a similar manner, without departing from structure of the invention or beyond the scope defined by this claim,
It is within the scope of protection of the invention.
Claims (10)
1. a kind of PET antibacterial matrices, which is characterized in that its raw material includes: 70-100 parts of PET resin, dispersing agent in parts by mass
1-5 parts, 1-8 parts of metal antibacterial agent, 5-10 parts of fire retardant, sisal fiber or modified sisal fiber 10-25 parts, coupling agent 0.1-
0.5 part.
2. PET antibacterial matrices as described in claim 1, which is characterized in that the dispersing agent include zinc stearate, polyethylene wax,
One of calcium stearate is a variety of.
3. PET antibacterial matrices as described in claim 1, which is characterized in that the coupling agent includes hexamethyldisilazane, diformazan
One of oxygroup dimethylsilane, phenyl triethoxysilane, gamma-mercaptopropyltriethoxysilane are a variety of.
4. PET antibacterial matrices as described in claim 1, which is characterized in that the metal antibacterial agent the preparation method comprises the following steps: press quality
Part weighs 5-10 parts of copper, 2-4 parts of zinc, 6-9 parts of silver, and mixed-powder is obtained after mixing；Anhydrous second is added into gained mixed-powder
Alcohol, N- aminoethyl-γ-aminopropyltrimethoxysilane, the mixed-powder, dehydrated alcohol, N- aminoethyl-γ-aminopropyl three
The mass ratio of methoxy silane is 1:(1-3): (0.05-0.1) obtains mixture, guarantor of the gained mixture in argon gas after being mixed
Shield is lower to carry out ultrasonic disperse processing, up to metal antibacterial agent after drying.
5. PET antibacterial matrices as described in claim 1, which is characterized in that the fire retardant includes diethyl zinc hypophosphite, trimerization
One of cyanamide phosphate, composite flame-retardant agent are a variety of.
6. PET antibacterial matrices as described in claim 1, which is characterized in that the modified sisal fiber is the preparation method comprises the following steps: by sisal hemp
In the ammonia spirit that it is 0.1-0.3mol/L to concentration that fiber, which is added, wherein the quality volume of the sisal fiber and ammonia spirit
Than obtaining mixture after ultrasonic treatment for 1:(1-5) (g/mL)；It is subsequently added into the plant extracts of mixture quality 1-3%, after
It is continuous to be ultrasonically treated, filtered fiber is obtained after filtering, and filtered fiber is washed with water, washing to neutrality,
Modified sisal fiber is obtained after drying.
7. PET antibacterial matrices as claimed in claim 5, which is characterized in that the composite flame-retardant agent is by weight percent by following
Raw material is prepared: triammonium phosphate 18-30%, barium metaborate 1-4%, magnesium hydroxide 6-12%, calcium oxide 1-3%, double seasons penta
Tetrol 8-15%, modifying agent 0.5-1.5%, surplus are ammonium polyphosphate.
8. PET antibacterial matrices as claimed in claim 6, which is characterized in that the plant extracts includes mint extract, bajiao banana
One of leaf extract, Eucalyptus extract are a variety of.
9. PET fire-retardant master granule as claimed in claim 7, which is characterized in that the composite flame-retardant agent the preparation method comprises the following steps: press quality
Percentage weighs each raw material component；First triammonium phosphate, ammonium polyphosphate are mixed, modifying agent is added after mixing, is placed in 50-95
It is stirred at DEG C, barium metaborate, magnesium hydroxide, calcium oxide, dipentaerythritol is added after mixing, after mixing to obtain the final product.
10. a kind of preparation method of PET antibacterial matrices as described in claim 1, which comprises the following steps:
I, weighs each raw material component by mass parts composition, obtains mixture after mixing；
Above-mentioned mixture feeding double screw extruder is granulated by II, obtains PET antibacterial matrices after cooling, drying.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111234270A (en) * | 2020-03-18 | 2020-06-05 | 百事基材料（青岛）股份有限公司 | Mint terylene master batch and preparation method thereof |
| CN114213709A (en) * | 2021-12-26 | 2022-03-22 | 上海帼帆化工新材料有限公司 | Antibacterial flame retardant, multifunctional antibacterial flame-retardant master batch, and preparation method and application thereof |
| US11566348B2 (en) * | 2019-11-06 | 2023-01-31 | Bestee Material (Tsingtao) Co., Ltd. | Method of preparing plant-based functional polyester filament |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1757672A (en) * | 2004-10-08 | 2006-04-12 | 上海毅兴塑胶原料有限公司 | Masterbatch used for processing polyester resin |
| CN101928448A (en) * | 2010-08-16 | 2010-12-29 | 中国科学技术大学 | Nano composite flame-retardant reinforced polyester engineering plastic and preparation method thereof |
| CN105820375A (en) * | 2016-05-23 | 2016-08-03 | 徐州猎奇商贸有限公司 | Composite flame retardant |
| CN106751554A (en) * | 2016-11-10 | 2017-05-31 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of sisal hemp reinforced polyester master batch and preparation method thereof |
-
2018
- 2018-08-30 CN CN201811002252.2A patent/CN109135208A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1757672A (en) * | 2004-10-08 | 2006-04-12 | 上海毅兴塑胶原料有限公司 | Masterbatch used for processing polyester resin |
| CN101928448A (en) * | 2010-08-16 | 2010-12-29 | 中国科学技术大学 | Nano composite flame-retardant reinforced polyester engineering plastic and preparation method thereof |
| CN105820375A (en) * | 2016-05-23 | 2016-08-03 | 徐州猎奇商贸有限公司 | Composite flame retardant |
| CN106751554A (en) * | 2016-11-10 | 2017-05-31 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of sisal hemp reinforced polyester master batch and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 于新等: "《天然食品添加剂》", 31 March 2014, 中国轻工业出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11566348B2 (en) * | 2019-11-06 | 2023-01-31 | Bestee Material (Tsingtao) Co., Ltd. | Method of preparing plant-based functional polyester filament |
| CN111234270A (en) * | 2020-03-18 | 2020-06-05 | 百事基材料（青岛）股份有限公司 | Mint terylene master batch and preparation method thereof |
| CN114213709A (en) * | 2021-12-26 | 2022-03-22 | 上海帼帆化工新材料有限公司 | Antibacterial flame retardant, multifunctional antibacterial flame-retardant master batch, and preparation method and application thereof |
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