CN109265933A - A kind of antibacterial PET composite material and preparation method - Google Patents
A kind of antibacterial PET composite material and preparation method Download PDFInfo
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- CN109265933A CN109265933A CN201810989325.5A CN201810989325A CN109265933A CN 109265933 A CN109265933 A CN 109265933A CN 201810989325 A CN201810989325 A CN 201810989325A CN 109265933 A CN109265933 A CN 109265933A
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Abstract
The present invention relates to a kind of antibacterial PET composite material and preparation methods, are made of the component of following parts by weight: PET is 80 parts -100 parts；Antibacterial agent is 4 parts -6 parts；Antioxidant is 0.1 part -0.5 part.The antibacterial agent formation mechenism of the application: pass through isopropyl three (dioctyl phosphoric acid acyloxy) modified TiO in titanate esters surface2Surface is rich in-NH2, surface is negatively charged, after being added in copper nitrate solution, due to attracting each other for positive and negative charge, Cu2+It will preferentially and NH2 ‑TiO is adsorbed on by electrostatic interaction2Surface, by the reduction of reducing agent 3-sec-butyl lithium borohydride, a large amount of copper particle is in TiO2Surface deposition, forms with TiO2For core, copper is the hud typed antibacterial agent of shell.
Description
Technical field
The invention belongs to technical field of polymer materials, particularly relate to a kind of antibacterial PET composite material and preparation method.
Background technique
Polyethylene terephthalate (PET) have it is light, nontoxic, odorless, chemical stability is good, and at normal temperature not
It is dissolved in common solvent, the advantages that water imbibition is small.Although the comprehensive performance of PET is very excellent, the anti-microbial property of PET is general,
Which greatly limits the application ranges of PET composite material.
Given this kind of reason, the anti-microbial property for improving PET with antibacterial agent of the technical program innovation, finally makes
A kind of PET composite material that anti-microbial property is excellent, make up the deficiency of existing PET composite material, this PET material is so far not yet
Report is seen, this has very important realistic meaning for the application of extension PET composite material.
Summary of the invention
The object of the present invention is to provide a kind of antibacterial PET composite material and preparation methods, compound to solve existing PET
The problem of material influences application range because anti-microbial property is not high.
The present invention is achieved by the following technical solutions:
A kind of antibacterial PET composite material, is made of the component of following parts by weight:
80 parts -100 parts of PET；
4 parts -6 parts of antibacterial agent；
0.1 part -0.5 part of antioxidant.
The preparation method of the antibacterial agent the following steps are included:
(1) a certain amount of copper nitrate solution, deionized water, ammonia spirit are weighed, they are sequentially added to reaction vessels
In, it is stirred to react 6-8h under room temperature and forms solution A；
(2) a certain amount of nano-TiO is weighed2, isopropyl three (dioctyl phosphoric acid acyloxy) titanate esters, deionized water, will
They are sequentially added into reaction vessels, are stirred to react 8-10h under room temperature, are obtained solution B；
(3) a certain amount of solution B, copper nitrate solution are weighed, they are sequentially added into reaction vessels, is stirred under room temperature
4-6h is reacted, solution C is obtained；
(4) it by solution C ultrasonic disperse 1-3h, is separated with centrifuge, removes upper layer supernatant liquid, filtered, washing, dry
Modified TiO2；
(5) a certain amount of modified TiO is weighed2, deionized water, 5- vinyl-2-pyrrolidone, three sec-butyl hydroborations
Lithium, potassium citrate, they are sequentially added into reaction vessels, are stirred to react 8-10h under room temperature, are obtained solution D；
(6) it by solution C ultrasonic disperse 1-3h, is separated with centrifuge, removes upper layer supernatant liquid, filtered, washing, dry
Powder E；
(7) a certain amount of powder E, solution A, formalin are weighed, they are sequentially added into reaction vessels, under room temperature
It is stirred to react 10-12h, obtains solution F；
(8) it by solution F ultrasonic disperse 2-4h, is separated with centrifuge, removes upper layer supernatant liquid, filtered, washed, it is dry,
500 meshes are crossed in grinding, both obtain antibacterial agent.
The mass ratio of copper nitrate solution, deionized water and ammonia spirit in step (1) is (10-16): (120-160):
(20-30)。
Nano-TiO in step (2)2, (the dioctyl phosphoric acid acyloxy) titanate esters of isopropyl three and deionized water quality
Than being (20-30): (1-3): (80-100).
The mass ratio of solution B and copper nitrate solution in step (3) is (60-80): (10-20).
Modification TiO in step (5)2, deionized water, 5- vinyl-2-pyrrolidone, 3-sec-butyl lithium borohydride and lemon
The mass ratio of lemon acid potassium is (30-40): (120-160): (3-5): (1-3): (2-4).
Powder E, solution A in step (7) and the mass ratio of formalin are (20-30): (60-80): (5-7).
The antioxidant is three (2,4- di-t-butyl) phenyl-phosphites, four [β-(3,5- di-tert-butyl-hydroxy phenyl)
Propionic acid] pentaerythritol ester or 1,3,5- trimethyls -2,4, one of 6- (3,5- di-t-butyl -4- hydroxyphenylmethyl) benzene or several
The mixing of kind.
The preparation method of any of the above-described antibacterial PET composite material, comprising the following steps:
(1) 80 parts -100 parts of PET, 4 parts of -6 parts of antibacterial agents, 0.1 part of -0.5 part of antioxidant is weighed to be mixed and stirred for uniformly,
Obtain mixture；
(2) by mixture extruding pelletization obtained in step (1) to get arrive PET composite material.
The step (2) specifically: mixture obtained in step (1) is put into the hopper of double screw extruder and squeezed
It is granulated out to get PET composite material is arrived, wherein the double screw extruder includes six humidity provinces sequentially arranged, area's temperature
240~260 DEG C of degree, two 280~300 DEG C of area's temperature, three 280~300 DEG C of area's temperature, four 280~300 DEG C of area's temperature, five area's temperature
280~300 DEG C of degree, six 280~300 DEG C of area's temperature, 280~300 DEG C of head temperature, 200~280r/min of screw speed.
The beneficial effects of the present invention are:
1, the antibacterial agent formation mechenism of the application: modified by (dioctyl phosphoric acid acyloxy) the titanate esters surface of isopropyl three
TiO afterwards2Surface is rich in-NH2, surface is negatively charged, after being added in copper nitrate solution, due to attracting each other for positive and negative charge,
Cu2+It will preferentially and NH2 -TiO is adsorbed on by electrostatic interaction2Surface, by the reduction of reducing agent 3-sec-butyl lithium borohydride, greatly
The copper particle of amount is in TiO2Surface deposition, forms with TiO2For core, copper is the hud typed antibacterial agent of shell.
2, PET composite material made from the application, anti-microbial property is excellent, compensates for the deficiency of existing product, has very big
Promotional value.
Specific embodiment
Carry out the technical solution that the present invention will be described in detail by the following examples, embodiment below is merely exemplary, only
It can be used to explanation and illustration technical solution of the present invention, and be not to be construed as the limitation to technical solution of the present invention.
Raw material used in embodiments herein is as follows:
PET (model 008L), Canadian Aclo；Copper nitrate solution, Jinan fly Chemical Co., Ltd.；Ammonia spirit, it is safe
Xing Sucheng Chemical Co., Ltd.；Deionized water, hundred Aurion of Beijing win Science and Technology Ltd.；Nano TiO 2, Beijing Deco Dao Jin section
Skill Co., Ltd；Isopropyl three (dioctyl phosphoric acid acyloxy) titanate esters, Hangzhou Jesse block Chemical Co., Ltd.；5- vinyl-
2-Pyrrolidone, Nanjing Ai Likaide Chemical Co., Ltd.；The auspicious limited public affairs of biotechnology are tieed up in 3-sec-butyl lithium borohydride, Jiangsu
Department；Potassium citrate, Wujiang south wind Fine Chemical Co., Ltd；Formalin, 100,000 Chemical Co., Ltd. of Shandong；Antioxidant (type
Number Irganox168, Irganox1010, Irganox1330), Switzerland's Ciba.
Test equipment used herein is as follows:
ZSK30 type double screw extruder, German W&P company；JL-1000 type tensile testing machine, the wide just experiment instrument in Guangzhou
The production of device company；HTL900-T-5B type injection (mo(u)lding) machine, the production of Hai Tai plastics machinery Co., Ltd；XCJ-500 type shock-testing
Machine, the production of Chengde testing machine factory；QT-1196 type tester for elongation, Dongguan City Gao Tai detecting instrument Co., Ltd；QD-GJS-
B12K type high-speed mixer, Beijing perseverance Order instrument and meter Co., Ltd.
The application provides a kind of antibacterial PET composite material, is made of the component of following parts by weight:
80 parts -100 parts of PET；
4 parts -6 parts of antibacterial agent；
0.1 part -0.5 part of antioxidant.
The preparation method of the antibacterial agent the following steps are included:
(1) a certain amount of copper nitrate solution, deionized water, ammonia spirit are weighed, they are sequentially added to reaction vessels
In, it is stirred to react 6-8h under room temperature and forms solution A；The mass ratio of copper nitrate solution, deionized water and ammonia spirit is (10-
16): (120-160): (20-30).
(2) a certain amount of nano-TiO is weighed2, isopropyl three (dioctyl phosphoric acid acyloxy) titanate esters, deionized water, will
They are sequentially added into reaction vessels, are stirred to react 8-10h under room temperature, are obtained solution B；Nano-TiO2, three (dioctyl of isopropyl
Phosphoric acid acyloxy) mass ratio of titanate esters and deionized water is (20-30): (1-3): (80-100).
(3) a certain amount of solution B, copper nitrate solution are weighed, they are sequentially added into reaction vessels, is stirred under room temperature
4-6h is reacted, solution C is obtained；The mass ratio of solution B and copper nitrate solution is (60-80): (10-20).
(4) it by solution C ultrasonic disperse 1-3h, is separated with centrifuge, removes upper layer supernatant liquid, filtered, washing, dry
Modified TiO2；
(5) a certain amount of modified TiO is weighed2, deionized water, 5- vinyl-2-pyrrolidone, three sec-butyl hydroborations
Lithium, potassium citrate, they are sequentially added into reaction vessels, are stirred to react 8-10h under room temperature, are obtained solution D；Modified TiO2、
Deionized water, 5- vinyl-2-pyrrolidone, 3-sec-butyl lithium borohydride and potassium citrate mass ratio be (30-40):
(120-160): (3-5): (1-3): (2-4).
(6) it by solution C ultrasonic disperse 1-3h, is separated with centrifuge, removes upper layer supernatant liquid, filtered, washing, dry
Powder E；
(7) a certain amount of powder E, solution A, formalin are weighed, they are sequentially added into reaction vessels, under room temperature
It is stirred to react 10-12h, obtains solution F；The mass ratio of powder E, solution A and formalin are (20-30): (60-80): (5-7).
(8) it by solution F ultrasonic disperse 2-4h, is separated with centrifuge, removes upper layer supernatant liquid, filtered, washed, it is dry,
500 meshes are crossed in grinding, both obtain antibacterial agent.
Antioxidant is three (2,4- di-t-butyl) phenyl-phosphites (abbreviation Irganox168), the four [β-of BASF AG
(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (abbreviation Irganox1010) and/or 1,3,5- trimethyl -2,
4,6- (3,5- di-t-butyl -4- hydroxyphenylmethyl) benzene are (referred to as
One or more of) Irganox1330 mixing.
The preparation method of any of the above-described antibacterial PET composite material, comprising the following steps:
(1) 80 parts -100 parts of PET, 4 parts of -6 parts of antibacterial agents, 0.1 part of -0.5 part of antioxidant is weighed to be mixed and stirred for uniformly,
Obtain mixture；
(2) by mixture extruding pelletization obtained in step (1) to get arrive PET composite material.
The step (2) specifically: mixture obtained in step (1) is put into the hopper of double screw extruder and squeezed
It is granulated out to get PET composite material is arrived, wherein the double screw extruder includes six humidity provinces sequentially arranged, area's temperature
240~260 DEG C of degree, two 280~300 DEG C of area's temperature, three 280~300 DEG C of area's temperature, four 280~300 DEG C of area's temperature, five area's temperature
280~300 DEG C of degree, six 280~300 DEG C of area's temperature, 280~300 DEG C of head temperature, 200~280r/min of screw speed.
Embodiment 1
(1) 80 parts of PET, 4 parts of antibacterial agents, 0.1 part of Irganox168 is weighed to be mixed and stirred for uniformly, obtaining mixture；
(2) by mixture extruding pelletization obtained in step (1) to get arrive PET composite material P1.
Wherein each area's temperature of double screw extruder and screw speed are respectively as follows: 240 DEG C of area's temperature, two 280 DEG C of area's temperature,
Three 280 DEG C of area's temperature, four 280 DEG C of area's temperature, five 280 DEG C of area's temperature, six 280 DEG C of area's temperature, 280 DEG C of head temperature, screw rod turns
Fast 200r/min.
Embodiment 2
(1) 100 parts of PET, 6 parts of antibacterial agents, 0.1 part of Irganox168,0.2 part of Irganox1010,0.2 part are weighed
Irganox1330 is mixed and stirred for uniformly, obtaining mixture；
(2) by mixture extruding pelletization obtained in step (1) to get arrive PET composite material P2.
Wherein each area's temperature of double screw extruder and screw speed are respectively as follows: 260 DEG C of area's temperature, two 300 DEG C of area's temperature,
Three 300 DEG C of area's temperature, four 300 DEG C of area's temperature, five 300 DEG C of area's temperature, six 300 DEG C of area's temperature, 300 DEG C of head temperature, screw rod turns
Fast 280r/min.
Embodiment 3
(1) 90 parts of PET, 5 parts of antibacterial agents, 0.1 part of Irganox168,0.2 part of Irganox1010 is weighed to be mixed and stirred for
It is even, obtain mixture；
(2) by mixture extruding pelletization obtained in step (1) to get arrive PET composite material P3.
Wherein each area's temperature of double screw extruder and screw speed are respectively as follows: 250 DEG C of area's temperature, two 290 DEG C of area's temperature,
Three 290 DEG C of area's temperature, four 290 DEG C of area's temperature, five 290 DEG C of area's temperature, six 290 DEG C of area's temperature, 290 DEG C of head temperature, screw rod turns
Fast 240r/min.
Embodiment 4
(1) 95 parts of PET, 5 parts of antibacterial agents, 0.1 part of Irganox1010,0.2 part of Irganox1330 is weighed to be mixed and stirred for
Uniformly, mixture is obtained；
(2) by mixture extruding pelletization obtained in step (1) to get arrive PET composite material P4.
Wherein each area's temperature of double screw extruder and screw speed are respectively as follows: 245 DEG C of area's temperature, two 285 DEG C of area's temperature,
Three 285 DEG C of area's temperature, four 285 DEG C of area's temperature, five 285 DEG C of area's temperature, six 285 DEG C of area's temperature, 285 DEG C of head temperature, screw rod turns
Fast 255r/min.
Embodiment 5
(1) 100 parts of PET, 4 parts of antibacterial agents, 0.2 part of Irganox1010,0.2 part of Irganox1330 is weighed to be mixed and stirred for
Uniformly, mixture is obtained；
(2) by mixture extruding pelletization obtained in step (1) to get arrive PET composite material P5.
Wherein each area's temperature of double screw extruder and screw speed are respectively as follows: 250 DEG C of area's temperature, two 295 DEG C of area's temperature,
Three 295 DEG C of area's temperature, four 295 DEG C of area's temperature, five 295 DEG C of area's temperature, six 295 DEG C of area's temperature, 295 DEG C of head temperature, screw rod turns
Fast 270r/min.
Comparative example 1
(1) 80 parts of PET, 0.1 part of Irganox1010,0.2 part of Irganox168 is weighed to be mixed and stirred for uniformly, being mixed
Close material；
(2) by mixture extruding pelletization obtained in step (1) to get arrive PET composite material D1.
Wherein each area's temperature of double screw extruder and screw speed are respectively as follows: 250 DEG C of area's temperature, two 295 DEG C of area's temperature,
Three 295 DEG C of area's temperature, four 295 DEG C of area's temperature, five 295 DEG C of area's temperature, six 295 DEG C of area's temperature, 295 DEG C of head temperature, screw rod turns
Fast 270r/min.
Performance test:
Batten test is made with injection molding machine in PET composite material prepared by above-described embodiment 1-5 and comparative example 1, tests number
According to being as follows:
As can be seen from the table, the antibiotic property of embodiment 1-5 will be better than comparative example 1, this illustrates the PET of the technical program
Composite material will be got well compared with the antibiotic property of common PET material.
A kind of PET composite material that anti-microbial property is very excellent has been made in the technical program, compensates for the deficiency of current material,
This greatly expands the application field of PET composite material, has great importance.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And deformation, the scope of the present invention are extremely equally limited by appended claims.
Claims (10)
1. a kind of antibacterial PET composite material, which is characterized in that be made of the component of following parts by weight:
80 parts -100 parts of PET；
4 parts -6 parts of antibacterial agent；
0.1 part -0.5 part of antioxidant.
2. antibacterial PET composite material according to claim 1, which is characterized in that the preparation method of the antibacterial agent includes
Following steps:
(1) a certain amount of copper nitrate solution, deionized water, ammonia spirit are weighed, they are sequentially added into reaction vessels, often
It is stirred to react 6-8h under temperature and forms solution A；
(2) a certain amount of nano-TiO is weighed2, isopropyl three (dioctyl phosphoric acid acyloxy) titanate esters, deionized water, by they according to
Secondary addition is stirred to react 8-10h under room temperature, obtains solution B into reaction vessels；
(3) a certain amount of solution B, copper nitrate solution are weighed, they are sequentially added into reaction vessels, is stirred to react under room temperature
4-6h obtains solution C；
(4) it by solution C ultrasonic disperse 1-3h, is separated with centrifuge, removes upper layer supernatant liquid, filtered, washing is modifiedly dry
TiO2；
(5) a certain amount of modified TiO is weighed2, deionized water, 5- vinyl-2-pyrrolidone, 3-sec-butyl lithium borohydride, lemon
Sour potassium, they are sequentially added into reaction vessels, are stirred to react 8-10h under room temperature, are obtained solution D；
(6) it by solution C ultrasonic disperse 1-3h, is separated with centrifuge, removes upper layer supernatant liquid, filtered, washing, dry powder
E；
(7) a certain amount of powder E, solution A, formalin are weighed, they are sequentially added into reaction vessels, is stirred under room temperature
10-12h is reacted, solution F is obtained；
(8) it by solution F ultrasonic disperse 2-4h, is separated with centrifuge, removes upper layer supernatant liquid, filtered, washed, dry, grinding,
500 meshes are crossed, antibacterial agent is both obtained.
3. antibacterial PET composite material according to claim 2, which is characterized in that copper nitrate solution in step (1) is gone
The mass ratio of ionized water and ammonia spirit is (10-16): (120-160): (20-30).
4. antibacterial PET composite material according to claim 2, which is characterized in that the nano-TiO in step (2)2, isopropyl
The mass ratio of three (dioctyl phosphoric acid acyloxy) titanate esters and deionized water is
(20-30): (1-3): (80-100).
5. antibacterial PET composite material according to claim 2, which is characterized in that solution B and copper nitrate in step (3)
The mass ratio of solution is (60-80): (10-20).
6. antibacterial PET composite material according to claim 2, which is characterized in that the modification TiO in step (5)2, deionization
Water, 5- vinyl-2-pyrrolidone, 3-sec-butyl lithium borohydride and potassium citrate mass ratio be (30-40): (120-160):
(3-5): (1-3): (2-4).
7. antibacterial PET composite material according to claim 2, which is characterized in that powder E, solution A in step (7) and
The mass ratio of formalin is (20-30): (60-80): (5-7).
8. antibacterial PET composite material according to claim 1, which is characterized in that the antioxidant is three (2,4- bis- tertiary fourths
Base) phenyl-phosphite, four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters or 1,3,5- trimethyl -2,
The mixing of one or more of 4,6- (3,5- di-t-butyl -4- hydroxyphenylmethyl) benzene.
9. the preparation method of any one of the claims 1 to 8 antibacterial PET composite material, which is characterized in that including following step
It is rapid:
(1) 80 parts -100 parts of PET, 4 parts of -6 parts of antibacterial agents, 0.1 part of -0.5 part of antioxidant is weighed to be mixed and stirred for uniformly, obtaining
Mixture；
(2) by mixture extruding pelletization obtained in step (1) to get arrive PET composite material.
10. the preparation method of antibacterial PET composite material according to claim 9, which is characterized in that step (2) tool
Body are as follows: it is compound to get PET is arrived that mixture obtained in step (1) is put into extruding pelletization in the hopper of double screw extruder
Material, wherein the double screw extruder includes six humidity provinces sequentially arranged, 240~260 DEG C of area's temperature, two area's temperature
280~300 DEG C of degree, three 280~300 DEG C of area's temperature, four 280~300 DEG C of area's temperature, five 280~300 DEG C of area's temperature, six area's temperature
280~300 DEG C of degree, 280~300 DEG C of head temperature, 200~280r/min of screw speed.
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| CN110117412A (en) * | 2019-04-02 | 2019-08-13 | 苏州海晨塑胶有限公司 | Antibacterial anti-oxidant polyester material of one kind and preparation method thereof |
| CN112266588A (en) * | 2020-10-30 | 2021-01-26 | 嘉兴高正新材料科技股份有限公司 | High-performance anti-aging PET composite material and preparation method thereof |
| CN115678104A (en) * | 2022-11-11 | 2023-02-03 | 安徽江淮汽车集团股份有限公司 | Preparation method of low-odor antibacterial filler and PET (polyethylene terephthalate) composite material containing low-odor antibacterial filler |
| CN115926391A (en) * | 2022-12-10 | 2023-04-07 | 重庆泛锐科技有限公司 | Antibacterial spray-free PET composite material and preparation method thereof |
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Address after: 230601 No. 99 Ziyun Road, Hefei Economic and Technological Development Zone, Anhui Province Applicant after: Anhui Jianghuai Automobile Group Limited by Share Ltd Address before: 230601 No. 669 Shixin Road, Taohua Industrial Park, Hefei City, Anhui Province Applicant before: Anhui Jianghuai Automobile Group Limited by Share Ltd |
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