CN117820820A - PET composite material and preparation method thereof - Google Patents
PET composite material and preparation method thereof Download PDFInfo
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- CN117820820A CN117820820A CN202211180375.1A CN202211180375A CN117820820A CN 117820820 A CN117820820 A CN 117820820A CN 202211180375 A CN202211180375 A CN 202211180375A CN 117820820 A CN117820820 A CN 117820820A
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- 239000002131 composite material Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 239000000835 fiber Substances 0.000 claims abstract description 54
- 239000003242 anti bacterial agent Substances 0.000 claims abstract description 45
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 30
- 150000002910 rare earth metals Chemical group 0.000 claims abstract description 30
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 10
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 239000000203 mixture Substances 0.000 claims description 26
- 239000008367 deionised water Substances 0.000 claims description 25
- 229910021641 deionized water Inorganic materials 0.000 claims description 25
- 238000006243 chemical reaction Methods 0.000 claims description 24
- 238000001354 calcination Methods 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 21
- 238000005406 washing Methods 0.000 claims description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- 239000010949 copper Substances 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 12
- 238000007873 sieving Methods 0.000 claims description 12
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 11
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 11
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 11
- 239000001099 ammonium carbonate Substances 0.000 claims description 11
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 claims description 11
- 229940069446 magnesium acetate Drugs 0.000 claims description 11
- 235000011285 magnesium acetate Nutrition 0.000 claims description 11
- 239000011654 magnesium acetate Substances 0.000 claims description 11
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 10
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 10
- 238000001125 extrusion Methods 0.000 claims description 10
- 238000005469 granulation Methods 0.000 claims description 10
- 230000003179 granulation Effects 0.000 claims description 10
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004599 antimicrobial Substances 0.000 claims 1
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 11
- 229920000139 polyethylene terephthalate Polymers 0.000 description 52
- 239000005020 polyethylene terephthalate Substances 0.000 description 52
- 238000001816 cooling Methods 0.000 description 10
- 238000005303 weighing Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 238000001291 vacuum drying Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 2
- 229920001661 Chitosan Polymers 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 244000179970 Monarda didyma Species 0.000 description 1
- 235000010672 Monarda didyma Nutrition 0.000 description 1
- -1 Polyethylene terephthalate Polymers 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011081 inoculation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000036314 physical performance Effects 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
The invention discloses a PET composite material and a preparation method thereof, wherein the PET composite material is prepared from 80-100 parts of PET, 10-20 parts of modified PBO fiber, 2-4 parts of antibacterial agent and 0.1-0.5 part of antioxidant according to parts by weight; wherein the modified PBO fiber is rare earth treated PBO fiber, and the antibacterial agent is nano MgO/Cu antibacterial agent. According to the invention, the newly developed nano MgO/Cu antibacterial agent is introduced into the PET system, so that the PET composite material has excellent antibacterial performance; meanwhile, rare earth treated PBO fibers are introduced into the PET system, so that the PET composite material is ensured to have excellent mechanical properties, and the application of the PET composite material can be greatly expanded.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a PET composite material and a preparation method thereof.
Background
Polyethylene terephthalate (PET) is a widely used high molecular polyester resin, and has the advantages of good fatigue resistance, good heat resistance, good dimensional stability and the like, but the physical properties and antibacterial properties of PET are general, which limits the application of PET composite materials in some specific fields.
The antibacterial performance of a PET system can be improved by adding a certain amount of antibacterial agent to the PET system, but the antibacterial performance of the traditional antibacterial agent has reached the bottleneck, and the invention aims to elucidate a PET composite material, wherein a novel antibacterial agent is added.
Disclosure of Invention
In view of the above, it is necessary to provide a PET composite material that has excellent antibacterial properties by introducing a newly developed nano MgO/Cu antibacterial agent into a PET system; meanwhile, rare earth treated PBO fiber is introduced into a PET system, so that the PET composite material is ensured to have excellent physical properties.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the invention provides a PET composite material which is prepared from 80-100 parts of PET, 10-20 parts of modified PBO fiber, 2-4 parts of antibacterial agent and 0.1-0.5 part of antioxidant according to parts by weight;
wherein the modified PBO fiber is rare earth treated PBO fiber, and the antibacterial agent is nano MgO/Cu antibacterial agent.
Further, the preparation of the modified PBO fiber comprises the following steps:
ce (NO) 3 ) 3 ·6H 2 Mixing O and ethanol uniformly to obtain a rare earth solution;
and mixing the PBO fiber, the rare earth solution and concentrated hydrochloric acid, reacting for 1-3 hours at 50-70 ℃, washing and drying to obtain the rare earth treated PBO fiber.
Further, the Ce (NO 3 ) 3 ·6H 2 The mass ratio of O to ethanol is (40-50): (180-240), wherein the concentration of the ethanol is 70% -80%.
Further, the mass ratio of the PBO fiber to the rare earth solution to the concentrated hydrochloric acid is (20-30): (160-180): (40-50).
Further, the preparation of the antibacterial agent comprises the following steps:
providing nano MgO;
mixing the nano MgO, copper nitrate and deionized water, stirring and reacting for 6-8 hours, and then filtering, washing, drying and calcining to obtain the nano MgO/Cu antibacterial agent.
Further, the preparation process of the nano MgO comprises the following steps:
mixing magnesium acetate, ammonium bicarbonate and deionized water, stirring at 60-80 ℃ for reaction for 8-10 hours, filtering, washing, drying, calcining and grinding, and sieving with a 800-mesh sieve to obtain nano MgO.
Further, in the preparation of nano MgO, the mass ratio of magnesium acetate, ammonium bicarbonate and deionized water is (20-30): (28-32): (120-160); the calcination temperature is 600-680 ℃ and the calcination time is 10-12h.
Further, the mass ratio of the nano MgO, the copper nitrate and the deionized water is (30-40): (32-36): (160-200); the calcination temperature is 560-600 ℃ and the calcination time is 8-10h.
Further, the antioxidant is at least one selected from the group consisting of antioxidant 168, antioxidant 1010 and antioxidant 1330.
The invention further provides a preparation method of the PET composite material, which comprises the following steps:
mixing PET, modified PBO fiber, an antibacterial agent and an antioxidant according to a proportion, and uniformly stirring to obtain a mixture;
adding the mixture into a double-screw extruder for extrusion granulation to obtain a PET composite material;
preferably, the twin-screw extruder comprises six temperature areas which are arranged in sequence, and the working temperatures of the twin-screw extruder are as follows: the first area is 240-260 ℃, the second area is 280-300 ℃, the third area is 280-300 ℃, the fourth area is 280-300 ℃, the fifth area is 280-300 ℃, the sixth area is 280-300 ℃, the temperature of the machine head is 280-300 ℃, and the screw rotating speed is 200-280r/min.
The invention has the following beneficial effects:
according to the invention, a newly synthesized nano MgO/Cu type antibacterial agent is added into the PET composite material, mgO is a traditional antibacterial material with good antibacterial performance, after copper is loaded, the antibacterial effect is greatly enhanced, and the antibacterial performance of the PET composite material can be improved.
Wherein, the synthesis equation of the antibacterial agent is as follows:
Mg(CH 3 COO) 2 +2NH 4 HCO 3 →2CH 3 COONH 4 +Mg(HCO 3 ) 2
Mg(HCO 3 ) 2 →MgO+2CO 2 +H 2 O
Cu(NO 3 ) 2 →Cu+O 2 +2NO 2 。
in addition, the rare earth treated PBO fiber is added in the PET composite material, and is modified by the rare earth solution, so that compared with the commercial PBO fiber, the PET composite material has better dispersibility, and the modified PET mechanical property is more excellent, so that the PET composite material has excellent mechanical property.
Detailed Description
The present invention will be illustrated by the following examples, which are given for illustrative purposes only and are not intended to limit the scope of the present invention in any way, and unless otherwise specified, the conditions or procedures not specifically described are conventional and the reagents and materials employed are commercially available. In the following examples and comparative examples, the "parts", etc. are parts by weight unless otherwise specified.
The raw materials used in the following examples are as follows:
PET (model 008L), aclo, canada; ethanol solution, jinan Ming chemical Co., ltd; PBO fiber, teron fiber technologies, inc. Of bergamot; magnesium acetate, shandong Hao chemical Co., ltd; copper nitrate, jinan Huijin chemical industry Co., ltd; ammonium bicarbonate, jinan De Qiao chemical technology Co., ltd; deionized water, beijing Bai Oy Lai Bo technology Co., ltd; ce (NO) 3 ) 3 ·6H 2 O，Shandong Desheng New Material Co., ltd; concentrated hydrochloric acid, a chemical industry company of Huafu, yangzhou.
In addition, the preparation processes in the following examples are conventional means in the art unless specifically described, and therefore, will not be described in detail; the parts in the following embodiments refer to parts by weight. The following antibacterial ratio test was conducted using test pieces of (50 mm.+ -. 2 mm) × (6 mm.+ -. 0.1 mm) specification, and after 24 hours of inoculation time.
Example 1
Preparation of modified PBO fibers
400g Ce (NO) was weighed 3 ) 3 ·6H 2 O, 1.8kg ethanol solution, ce (NO 3 ) 3 ·6H 2 Adding O into ethanol solution to prepare rare earth solution;
200g of PBO fiber and 1.6kg of rare earth solution are put into a beaker containing 400g of concentrated hydrochloric acid, the beaker is placed into a water bath kettle with the temperature of 50 ℃ for reaction for 1h, and then deionized water is used for washing the surface until the pH=7; and then drying the fiber in a vacuum drying oven at 60 ℃ for 2 hours to obtain the PBO fiber treated by the rare earth solution, which is denoted as modified PBO fiber N1.
Preparation of nano MgO/Cu antibacterial agent
200g of magnesium acetate, 280g of ammonium bicarbonate and 1.2kg of deionized water are weighed, added into a reaction vessel and stirred for reaction for 8 hours at 60 ℃; then filtering, washing and drying, then placing the mixture into a muffle furnace at 600 ℃ for calcination for 10 hours, cooling, grinding and sieving with a 800-mesh sieve to obtain nano MgO;
weighing 300g of nano MgO, 320g of copper nitrate and 1.6kg of deionized water, adding the materials into a reaction vessel, and stirring and reacting for 6 hours at normal temperature; and then filtering, washing and drying, placing into a muffle furnace at 560 ℃ for calcination for 8 hours, cooling, grinding and sieving with a 800-mesh sieve to obtain the nano MgO/Cu antibacterial agent, which is marked as an antibacterial agent Q1.
Preparation of PET composite material
Weighing 80 parts of PET, 10 parts of modified PBO fiber N1, 2 parts of antibacterial agent Q1 and 0.1 part of antioxidant 1010 according to the total parts, mixing and stirring uniformly to obtain a mixture;
and adding the obtained mixture into a double-screw extruder for extrusion granulation to obtain the PET composite material, which is denoted as P1.
Wherein, each district temperature and screw rod rotational speed of twin-screw extruder are respectively: the temperature of the first area is 240 ℃, the temperature of the second area is 280 ℃, the temperature of the third area is 280 ℃, the temperature of the fourth area is 280 ℃, the temperature of the fifth area is 280 ℃, the temperature of the sixth area is 280 ℃, the temperature of the machine head is 280 ℃, and the rotating speed of the screw is 200r/min.
Example 2
Preparation of modified PBO fibers
500g Ce (NO) was weighed 3 ) 3 ·6H 2 O, 2.4kg ethanol solution, ce (NO 3 ) 3 ·6H 2 Adding O into ethanol solution to prepare rare earth solution;
300g of PBO fiber and 1.8kg of rare earth solution are put into a beaker containing 500g of concentrated hydrochloric acid, the beaker is put into a water bath kettle with the temperature of 70 ℃ for reaction for 3 hours, and then deionized water is used for washing the surface until the pH=7; and then drying for 4 hours in a vacuum drying oven at 80 ℃ to obtain the PBO fiber treated by the rare earth solution, which is denoted as modified PBO fiber N2.
Preparation of nano MgO/Cu antibacterial agent
300g of magnesium acetate, 320g of ammonium bicarbonate and 1.6kg of deionized water are weighed, added into a reaction vessel and stirred for reaction for 10 hours at 80 ℃; then filtering, washing and drying, then placing the mixture into a muffle furnace at 680 ℃ for calcining for 12 hours, cooling, grinding and sieving with a 800-mesh sieve to obtain nano MgO;
400g of nano MgO, 360g of copper nitrate and 2.0kg of deionized water are weighed, added into a reaction vessel and stirred at normal temperature for reaction for 8 hours; then filtering, washing, drying, placing into a muffle furnace at 600 ℃ for calcination for 10 hours, cooling, grinding and sieving with a 800-mesh sieve to obtain the nano MgO/Cu antibacterial agent, which is marked as an antibacterial agent Q2.
Preparation of PET composite material
Weighing 100 parts of PET, 20 parts of modified PBO fiber N2, 4 parts of antibacterial agent Q2, 0.1 part of antioxidant 1010 and 0.2 part of antioxidant 168 according to the total parts, mixing and stirring uniformly to obtain a mixture;
and adding the obtained mixture into a double-screw extruder for extrusion granulation to obtain the PET composite material, which is marked as P2.
Wherein, each district temperature and screw rod rotational speed of twin-screw extruder are respectively: the temperature of the first area is 260 ℃, the temperature of the second area is 300 ℃, the temperature of the third area is 300 ℃, the temperature of the fourth area is 300 ℃, the temperature of the fifth area is 300 ℃, the temperature of the sixth area is 300 ℃, the temperature of the machine head is 300 ℃, and the rotating speed of the screw is 280r/min.
Example 3
Preparation of modified PBO fibers
Weigh 450g Ce (NO) 3 ) 3 ·6H 2 O, 2.1kg ethanol solution, ce (NO 3 ) 3 ·6H 2 Adding O into ethanol solution to prepare rare earth solution;
putting 250g of PBO fiber and 1.7kg of rare earth solution into a beaker containing 450g of concentrated hydrochloric acid, putting the beaker into a water bath kettle at 60 ℃ for reaction for 2 hours, and then washing the surface with deionized water until the pH=7; and then drying for 3 hours in a vacuum drying oven at 70 ℃ to obtain the PBO fiber treated by the rare earth solution, which is denoted as modified PBO fiber N3.
Preparation of nano MgO/Cu antibacterial agent
250g of magnesium acetate, 300g of ammonium bicarbonate and 1.4kg of deionized water are weighed, added into a reaction vessel and stirred for reaction for 9 hours at 70 ℃; then filtering, washing and drying, then placing the mixture into a muffle furnace at 640 ℃ for calcining for 11 hours, cooling, grinding and sieving with a 800-mesh sieve to obtain nano MgO;
weighing 350g of nano MgO, 340g of copper nitrate and 1.8kg of deionized water, adding the materials into a reaction vessel, and stirring and reacting for 7 hours at normal temperature; and then filtering, washing and drying, placing into a muffle furnace at 580 ℃ for calcination for 9 hours, cooling, grinding and sieving with a 800-mesh sieve to obtain the nano MgO/Cu antibacterial agent, which is denoted as an antibacterial agent Q3.
Preparation of PET composite material
90 parts of PET, 15 parts of modified PBO fiber N3, 3 parts of antibacterial agent Q3, 0.1 part of antioxidant 168 and 0.2 part of antioxidant 1010 are weighed according to the total parts, mixed and stirred uniformly to obtain a mixture;
and adding the obtained mixture into a double-screw extruder for extrusion granulation to obtain the PET composite material, which is marked as P3.
Wherein, each district temperature and screw rod rotational speed of twin-screw extruder are respectively: the temperature of the first area is 250 ℃, the temperature of the second area is 290 ℃, the temperature of the third area is 290 ℃, the temperature of the fourth area is 290 ℃, the temperature of the fifth area is 290 ℃, the temperature of the sixth area is 290 ℃, the temperature of the machine head is 290 ℃, and the rotating speed of the screw is 240r/min.
Example 4
Preparation of modified PBO fibers
480g Ce (NO) was weighed 3 ) 3 ·6H 2 O, 1.95kg ethanol solution, ce (NO 3 ) 3 ·6H 2 Adding O into ethanol solution to prepare rare earth solution;
280g of PBO fiber and 1.75kg of rare earth solution are put into a beaker containing 420g of concentrated hydrochloric acid, the beaker is placed into a water bath kettle with the temperature of 55 ℃ for reaction for 3 hours, and then deionized water is used for washing the surface until the pH=7; and drying the fiber in a vacuum drying oven at 65 ℃ for 2 hours to obtain the PBO fiber treated by the rare earth solution, which is denoted as modified PBO fiber N4.
Preparation of nano MgO/Cu antibacterial agent
Weighing 210g of magnesium acetate, 290g of ammonium bicarbonate and 1.3kg of deionized water, adding the magnesium acetate, the 290g of ammonium bicarbonate and the 1.3kg of deionized water into a reaction vessel, and stirring and reacting for 8 hours at 65 ℃; then filtering, washing and drying, then placing the mixture into a muffle furnace at 670 ℃ for calcining for 11 hours, cooling, grinding and sieving with a 800-mesh sieve to obtain nano MgO;
330g of nano MgO, 350g of copper nitrate and 1.9kg of deionized water are weighed, added into a reaction vessel and stirred at normal temperature for reaction for 7 hours; and then filtering, washing and drying, placing into a muffle furnace at 590 ℃ for calcination for 9 hours, cooling, grinding and sieving with a 800-mesh sieve to obtain the nano MgO/Cu antibacterial agent, which is denoted as an antibacterial agent Q4.
Preparation of PET composite material
Weighing 95 parts of PET, 11 parts of modified PBO fiber N4, 4 parts of antibacterial agent Q4, 0.1 part of antioxidant 1010 and 0.2 part of antioxidant 1330 according to the total parts, mixing and uniformly stirring to obtain a mixture;
and adding the obtained mixture into a double-screw extruder for extrusion granulation to obtain the PET composite material, which is marked as P4.
Wherein, each district temperature and screw rod rotational speed of twin-screw extruder are respectively: the temperature of the first zone is 245 ℃, the temperature of the second zone is 285 ℃, the temperature of the third zone is 285 ℃, the temperature of the fourth zone is 285 ℃, the temperature of the fifth zone is 285 ℃, the temperature of the sixth zone is 285 ℃, the temperature of the machine head is 285 ℃, and the rotating speed of the screw is 210r/min.
Example 5
Preparation of modified PBO fibers
Weigh 430g Ce (NO) 3 ) 3 ·6H 2 O, 2.2kg ethanol solution, ce (NO 3 ) 3 ·6H 2 Adding O into ethanol solution to prepare rare earth solution;
290g of PBO fiber and 1.65kg of rare earth solution are put into a beaker containing 490g of concentrated hydrochloric acid, the beaker is put into a water bath kettle with the temperature of 55 ℃ for reaction for 3 hours, and then deionized water is used for washing the surface until the pH=7; and then drying for 4 hours in a vacuum drying oven at 75 ℃ to obtain the PBO fiber treated by the rare earth solution, which is denoted as modified PBO fiber N5.
Preparation of nano MgO/Cu antibacterial agent
260g of magnesium acetate, 315g of ammonium bicarbonate and 1.5kg of deionized water are weighed, added into a reaction vessel and stirred for reaction for 10 hours at 65 ℃; then filtering, washing and drying, then placing the mixture into a muffle furnace at 675 ℃ for calcination for 10 hours, cooling, grinding and sieving the mixture with a 800-mesh sieve to obtain nano MgO;
390g of nano MgO, 355g of copper nitrate and 1.85kg of deionized water are weighed, added into a reaction vessel and stirred at normal temperature for reaction for 8 hours; and then filtering, washing and drying, placing into a muffle furnace at 580 ℃ for calcination for 9 hours, cooling, grinding and sieving with a 800-mesh sieve to obtain the nano MgO/Cu antibacterial agent, which is denoted as an antibacterial agent Q5.
Preparation of PET composite material
Weighing 95 parts of PET, 12 parts of modified PBO fiber N5, 2 parts of antibacterial agent Q5, 0.1 part of antioxidant 1010 and 0.1 part of antioxidant 168 according to the total parts, mixing and stirring uniformly to obtain a mixture;
and adding the obtained mixture into a double-screw extruder for extrusion granulation to obtain the PET composite material, which is marked as P5.
Wherein, each district temperature and screw rod rotational speed of twin-screw extruder are respectively: the temperature of the first area is 245 ℃, the temperature of the second area is 295 ℃, the temperature of the third area is 295 ℃, the temperature of the fourth area is 295 ℃, the temperature of the fifth area is 295 ℃, the temperature of the sixth area is 295 ℃, the temperature of the machine head is 295 ℃, and the rotating speed of the screw is 270r/min.
Comparative example 1
Weighing 95 parts of PET, 0.1 part of antioxidant 1010 and 0.1 part of antioxidant 168 according to the total parts, mixing and stirring uniformly to obtain a mixture;
and adding the obtained mixture into a double-screw extruder for extrusion granulation to obtain the PET composite material, which is marked as D1.
Wherein, each district temperature and screw rod rotational speed of twin-screw extruder are respectively: the temperature of the first area is 245 ℃, the temperature of the second area is 295 ℃, the temperature of the third area is 295 ℃, the temperature of the fourth area is 295 ℃, the temperature of the fifth area is 295 ℃, the temperature of the sixth area is 295 ℃, the temperature of the machine head is 295 ℃, and the rotating speed of the screw is 270r/min.
Comparative example 2
Weighing 95 parts of PET, 12 parts of modified PBO fiber N5, 2 parts of antimicrobial chitosan micropowder, 0.1 part of antioxidant 1010 and 0.1 part of antioxidant 168 according to the total parts, mixing and stirring uniformly to obtain a mixture;
and adding the obtained mixture into a double-screw extruder for extrusion granulation to obtain the PET composite material, which is marked as D2.
Wherein, each district temperature and screw rod rotational speed of twin-screw extruder are respectively: the temperature of the first area is 245 ℃, the temperature of the second area is 295 ℃, the temperature of the third area is 295 ℃, the temperature of the fourth area is 295 ℃, the temperature of the fifth area is 295 ℃, the temperature of the sixth area is 295 ℃, the temperature of the machine head is 295 ℃, and the rotating speed of the screw is 270r/min.
Comparative example 3
Weighing 95 parts of PET, 12 parts of PBO fiber, 2 parts of antibacterial agent Q5, 0.1 part of antioxidant 1010 and 0.1 part of antioxidant 168 according to the total parts, mixing and stirring uniformly to obtain a mixture;
and adding the obtained mixture into a double-screw extruder for extrusion granulation to obtain the PET composite material, which is marked as D2.
Wherein, each district temperature and screw rod rotational speed of twin-screw extruder are respectively: the temperature of the first area is 245 ℃, the temperature of the second area is 295 ℃, the temperature of the third area is 295 ℃, the temperature of the fourth area is 295 ℃, the temperature of the fifth area is 295 ℃, the temperature of the sixth area is 295 ℃, the temperature of the machine head is 295 ℃, and the rotating speed of the screw is 270r/min.
Comparative example 4
The present comparative example uses the same embodiment as in example 5, except that: in the preparation of the PET composite, 2 parts of the antibacterial agent Q5 was replaced with 2 parts of nano MgO, and the other components were the same as in example 5.
Comparative example 5
The present comparative example uses the same embodiment as in example 5, except that: in the preparation of the PET composite, 2 parts of the antibacterial agent Q5 was replaced with 2 parts of the copper ion antibacterial agent, and the same as in example 5 was repeated.
Test case
The PET composites prepared in examples and comparative examples were subjected to the test for the relevant properties, and the results are shown in Table 1.
Table 1 results of PET composite Performance test
From the test results in table 1, it can be seen that the antibacterial performance and physical performance of examples 1 to 5 are better in combination, which illustrates that the PET composite material prepared by the method provided by the invention is excellent in combination performance, and the application field of the PET composite material can be expanded.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (10)
1. The PET composite material is characterized by being prepared from 80-100 parts of PET, 10-20 parts of modified PBO fiber, 2-4 parts of antibacterial agent and 0.1-0.5 part of antioxidant according to parts by weight;
wherein the modified PBO fiber is rare earth treated PBO fiber, and the antibacterial agent is nano MgO/Cu antibacterial agent.
2. The PET composite of claim 1 wherein the preparation of the modified PBO fibers comprises the steps of:
ce (NO) 3 ) 3 ·6H 2 Mixing O and ethanol uniformly to obtain a rare earth solution;
and mixing the PBO fiber, the rare earth solution and concentrated hydrochloric acid, reacting for 1-3 hours at 50-70 ℃, washing and drying to obtain the rare earth treated PBO fiber.
3. The PET composite of claim 2, wherein the Ce (NO 3 ) 3 ·6H 2 The mass ratio of O to ethanol is (40-50): (180-240), wherein the concentration of the ethanol is 70% -80%.
4. The PET composite material of claim 2, wherein the PBO fiber, rare earth solution and concentrated hydrochloric acid have a mass ratio of (20-30): (160-180): (40-50).
5. The PET composite of claim 1, wherein the preparation of the antimicrobial agent comprises the steps of:
providing nano MgO;
mixing the nano MgO, copper nitrate and deionized water, stirring and reacting for 6-8 hours, and then filtering, washing, drying and calcining to obtain the nano MgO/Cu antibacterial agent.
6. The PET composite material of claim 5, wherein the nano MgO is prepared by the process comprising:
mixing magnesium acetate, ammonium bicarbonate and deionized water, stirring at 60-80 ℃ for reaction for 8-10 hours, filtering, washing, drying, calcining and grinding, and sieving with a 800-mesh sieve to obtain nano MgO.
7. The PET composite material according to claim 6, wherein in the preparation of nano MgO, the mass ratio of magnesium acetate, ammonium bicarbonate and deionized water is (20-30): (28-32): (120-160); the calcination temperature is 600-680 ℃ and the calcination time is 10-12h.
8. The PET composite material of claim 5, wherein the mass ratio of nano MgO, copper nitrate, deionized water is (30-40): (32-36): (160-200); the calcination temperature is 560-600 ℃ and the calcination time is 8-10h.
9. The PET composite of claim 1, wherein the antioxidant is selected from at least one of antioxidant 168, antioxidant 1010, antioxidant 1330.
10. A process for the preparation of a PET composite material according to any one of claims 1 to 9, comprising the steps of:
mixing PET, modified PBO fiber, an antibacterial agent and an antioxidant according to a proportion, and uniformly stirring to obtain a mixture;
adding the mixture into a double-screw extruder for extrusion granulation to obtain a PET composite material;
preferably, the twin-screw extruder comprises six temperature areas which are arranged in sequence, and the working temperatures of the twin-screw extruder are as follows: the first area is 240-260 ℃, the second area is 280-300 ℃, the third area is 280-300 ℃, the fourth area is 280-300 ℃, the fifth area is 280-300 ℃, the sixth area is 280-300 ℃, the temperature of the machine head is 280-300 ℃, and the screw rotating speed is 200-280r/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211180375.1A CN117820820A (en) | 2022-09-27 | 2022-09-27 | PET composite material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211180375.1A CN117820820A (en) | 2022-09-27 | 2022-09-27 | PET composite material and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN117820820A true CN117820820A (en) | 2024-04-05 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202211180375.1A Pending CN117820820A (en) | 2022-09-27 | 2022-09-27 | PET composite material and preparation method thereof |
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| Country | Link |
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| CN (1) | CN117820820A (en) |
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- 2022-09-27 CN CN202211180375.1A patent/CN117820820A/en active Pending
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