CN114044969B - Highlight antibacterial PP composite material and preparation method thereof - Google Patents
Highlight antibacterial PP composite material and preparation method thereof Download PDFInfo
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- CN114044969B CN114044969B CN202111263311.3A CN202111263311A CN114044969B CN 114044969 B CN114044969 B CN 114044969B CN 202111263311 A CN202111263311 A CN 202111263311A CN 114044969 B CN114044969 B CN 114044969B
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention discloses a highlight antibacterial PP composite material and a preparation method thereof, wherein the highlight antibacterial PP composite material is prepared from the following components in parts by weight: 100 parts of PP, 6-10 parts of modified barium sulfate and 0.1-0.5 part of antioxidant. The modified barium sulfate is modified by adopting N-2-aminoethyl-3-aminopropyl trimethoxy silane, the hydrophilicity of the barium sulfate is changed into hydrophobicity, and then the reducing agent glucose is utilized to successfully prepare the copper-loaded barium sulfate with good antibacterial performance; meanwhile, after the barium sulfate is modified by the N-2-aminoethyl-3-aminopropyl trimethoxy silane, the dispersibility is good, and the glossiness of the PP composite material can be improved due to the high barium content and high whiteness of the barium sulfate. The PP composite material prepared by the invention has high gloss, good antibacterial property and excellent mechanical property, and the application range of the PP composite material is enlarged.
Description
Technical Field
The invention belongs to the field of high polymer materials, and particularly relates to a highlight antibacterial PP composite material and a preparation method thereof.
Background
The polypropylene (PP) has the advantages of light weight, no toxicity, no odor, good chemical stability, small water absorption, and the like. Although the overall properties of PP are very excellent, PP is required to have higher gloss and better antimicrobial properties in some fields.
For this reason, the novel PP composite material with excellent high light performance and antibacterial performance is innovatively used, so that the defects of the existing PP composite material are overcome, and the application of the PP composite material is expanded.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a highlight antibacterial PP composite material and a preparation method thereof, wherein the PP composite material has good highlight performance and antibacterial performance, and solves the technical problems of the prior art that the PP highlight performance and the antibacterial performance are limited.
The aim of the invention is realized by the following technical scheme:
the highlight antibacterial PP composite material is prepared from the following components in parts by weight:
PP100 parts
6-10 parts of modified barium sulfate
0.1 to 0.5 part of antioxidant
The modified barium sulfate is prepared by the following steps:
(1) Dispersing barium sulfate in the dispersion liquid, adding N-2-aminoethyl-3-aminopropyl trimethoxysilane, and stirring at 40-60 ℃ for reaction for 6-8h to form a mixed liquid A; further, the dispersion liquid is a mixed liquid of absolute ethyl alcohol and deionized water; the mass ratio of the barium sulfate, the absolute ethyl alcohol, the deionized water and the N-2-aminoethyl-3-aminopropyl trimethoxysilane is (40-50): (60-80): (120-160): (0.1-0.3).
(2) Filtering the mixed solution A to obtain a solid substance, and washing and drying the solid substance in sequence to obtain the modified barium sulfate B.
(3) Mixing modified barium sulfate B, copper salt, reducing agent glucose and deionized water, adding into a reaction vessel, placing the reaction vessel into a microwave reactor, and carrying out reduction reaction for 6-8h to obtain a mixed solution C. Further, the mass ratio of the modified barium sulfate B to the copper salt to the reducing agent glucose to the deionized water is (30-40): (10-16): (1-3): (100-160); the copper salt is copper nitrate, copper sulfate or copper phosphate; the power of the microwave reactor is 550-750W, the microwave reactor has more accurate temperature and reaction process control effect than the conventional reactor, the uniformity and consistency of the synthesis reaction are ensured, and the experimental efficiency is improved.
(4) And (3) performing ultrasonic dispersion on the mixed solution C for 4-6 hours, and sequentially performing centrifugal separation, filtration, washing and drying to obtain the modified barium sulfate.
As a preferable technical scheme, the antioxidant is at least one of tri (2, 4-di-tert-butyl) phenyl phosphite (Irganox 168 for short), tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester (Irganox 1010 for short) and 1,3, 5-trimethyl-2, 4,6- (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene (Irganox 1330 for short).
The invention also provides a preparation method of the highlight antibacterial PP composite material, which comprises the following steps:
(1) Weighing 100 parts of PP, 6-10 parts of modified barium sulfate and 0.1-0.5 part of antioxidant, mixing and stirring uniformly to obtain a mixture;
(2) Putting the mixture obtained in the step (1) into a hopper of a double-screw extruder for extrusion granulation to obtain the PP composite material; the double-screw extruder comprises six temperature areas which are sequentially arranged, and the temperatures of the areas are respectively as follows: the temperature of the first area is 180-200 ℃, the temperature of the second area is 220-240 ℃, the temperature of the third area is 220-240 ℃, the temperature of the fourth area is 220-240 ℃, the temperature of the fifth area is 220-240 ℃, and the temperature of the sixth area is 220-240 ℃; the temperature of the head of the double-screw extruder is 220-240 ℃ and the screw rotating speed is 200-280 r/min.
Compared with the prior art, the invention has the beneficial effects that:
the barium sulfate of the present invention acts in two ways: on the one hand, the barium content in the barium sulfate is high, the whiteness is high, and the glossiness of the PP composite material can be improved. On the other hand, the N-2-aminoethyl-3-aminopropyl trimethoxy silane is adopted to modify barium sulfate, the barium sulfate is changed from hydrophilicity to hydrophobicity, and then the reducing agent glucose is utilized to successfully prepare the copper-loaded barium sulfate with good antibacterial performance, so that the antibacterial property of the PP composite material can be well improved.
The barium sulfate in the patent has good dispersibility after being modified by the N-2-aminoethyl-3-aminopropyl trimethoxy silane, and can obtain higher Gao Ze degrees when being used for modifying PP; the PP composite material prepared by the invention has high gloss and good antibacterial property, and the application range of the PP composite material is enlarged.
Detailed Description
In order that the invention may be readily understood, a more complete description of the invention will be rendered by reference to specific embodiments that are now described. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The raw materials used in the following examples are as follows:
PP (model EP 649N), korean dalin; barium sulfate, gallery blue chemical Co., ltd; absolute ethanol, wuhanxiang he yi chemical technology limited; copper nitrate, henan Paddy chemical industry; glucose, jinan Osli chemical Co., ltd; n-2-aminoethyl-3-aminopropyl trimethoxysilane, nanjing austempered chemical industry; deionized water, shanghai Union test chemical reagents, inc.; antioxidants (model Irganox168, irganox1010, irganox 1330), basf, germany.
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 antibacterial rate test of the following examples and comparative examples was carried out using test pieces of the specification (50 mm.+ -. 2 mm) × (2 mm.+ -. 0.1 mm) after 24 hours of inoculation time. The tensile bars used for the tensile strength test have a model number of (170.0+ -5.0) mm (10.0+ -0.5) mm (4.0+ -0.2) mm and a tensile rate of 50mm/min; the cantilever beam notch impact strength spline used for the cantilever beam notch impact strength test has the following model: (80.0+ -5.0) mm (10.0+ -0.5) mm (4.0+ -0.2) mm, notch machined, notch depth (2.0+ -0.2) mm.
Preparation example 1
(1) 400g of barium sulfate, 600g of absolute ethyl alcohol, 1.2kg of deionized water and 1g of N-2-aminoethyl-3-aminopropyl trimethoxysilane are weighed, added into a reaction vessel and stirred at 40 ℃ for reaction for 6 hours to form a mixed solution A.
(2) And filtering, washing and drying the mixed solution A to obtain the modified barium sulfate B.
(3) 300g of modified barium sulfate B, 100g of copper nitrate, 10g of reducing agent glucose and 1.0kg of deionized water are weighed, sequentially added into a reaction vessel, the reaction vessel is placed into a microwave reactor, the power of the microwave reactor is 550W, and the reduction reaction is carried out for 6 hours, so that a mixed solution C is obtained.
(4) And (3) performing ultrasonic dispersion on the mixed solution C for 4 hours, separating by using a centrifugal machine, filtering, washing and drying to obtain the modified barium sulfate M1.
Example 1
(1) 100 parts of PP, 6 parts of modified barium sulfate M1 and 0.1 part of Irganox168 are weighed, mixed and stirred uniformly to obtain a mixture;
(2) And (3) extruding and granulating the mixture obtained in the step (1) to obtain the PP composite material P1.
Wherein the temperature and the screw rotating speed of each zone of the double-screw extruder are respectively as follows: 180 ℃ in the first area, 220 ℃ in the second area, 220 ℃ in the third area, 220 ℃ in the fourth area, 220 ℃ in the fifth area, 220 ℃ in the sixth area, 220 ℃ in the head and 200r/min of screw speed.
Preparation example 2
(1) 500g of barium sulfate, 800g of absolute ethyl alcohol, 1.6kg of deionized water and 3g of N-2-aminoethyl-3-aminopropyl trimethoxysilane are weighed, added into a reaction vessel and stirred at 60 ℃ for reaction for 8 hours to form a mixed solution A.
(2) And filtering, washing and drying the mixed solution A to obtain the modified barium sulfate B.
(3) 400g of modified barium sulfate B, 160g of copper nitrate, 30g of reducing agent glucose and 1.6kg of deionized water are weighed, sequentially added into a reaction vessel, the reaction vessel is placed into a microwave reactor, the power of the microwave reactor is 750W, and the reduction reaction is carried out for 8 hours, so that a mixed solution C is obtained.
(4) And (3) performing ultrasonic dispersion on the mixed solution C for 6 hours, separating by using a centrifugal machine, filtering, washing and drying to obtain the modified barium sulfate M2.
Example 2
(1) 100 parts of PP, 10 parts of modified barium sulfate M2, 0.1 part of Irganox168, 0.2 part of Irganox1010 and 0.2 part of Irganox1330 are weighed and mixed uniformly to obtain a mixture;
(2) And (3) extruding and granulating the mixture obtained in the step (1) to obtain the PP composite material P2.
Wherein the temperature and the screw rotating speed of each zone of the double-screw extruder are respectively as follows: the temperature of the first area is 200 ℃, the temperature of the second area is 240 ℃, the temperature of the third area is 240 ℃, the temperature of the fourth area is 240 ℃, the temperature of the fifth area is 240 ℃, the temperature of the sixth area is 240 ℃, the temperature of the machine head is 240 ℃, and the rotating speed of the screw is 280r/min.
Preparation example 3
(1) 450g of barium sulfate, 700g of absolute ethyl alcohol, 1.4kg of deionized water and 2g of N-2-aminoethyl-3-aminopropyl trimethoxysilane are weighed, added into a reaction vessel and stirred at 50 ℃ for reaction for 7 hours to form a mixed solution A.
(2) And filtering, washing and drying the mixed solution A to obtain the modified barium sulfate B.
(3) 350g of modified barium sulfate B, 130g of copper nitrate, 20g of reducing agent glucose and 1.3kg of deionized water are weighed, sequentially added into a reaction vessel, the reaction vessel is placed into a microwave reactor, the power of the microwave reactor is 700W, and the reduction reaction is carried out for 7 hours, so that a mixed solution C is obtained.
(4) And (3) performing ultrasonic dispersion on the mixed solution C for 5 hours, separating by using a centrifugal machine, filtering, washing and drying to obtain the modified barium sulfate M3.
Example 3
(1) 100 parts of PP, 8 parts of modified barium sulfate M3, 0.1 part of Irganox168 and 0.2 part of Irganox1010 are weighed and mixed uniformly to obtain a mixture;
(2) And (3) extruding and granulating the mixture obtained in the step (1) to obtain the PP composite material P3.
Wherein the temperature and the screw rotating speed of each zone of the double-screw extruder are respectively as follows: the temperature of the first area is 190 ℃, the temperature of the second area is 230 ℃, the temperature of the third area is 230 ℃, the temperature of the fourth area is 230 ℃, the temperature of the fifth area is 230 ℃, the temperature of the sixth area is 230 ℃, the temperature of the machine head is 230 ℃, and the rotating speed of the screw is 240r/min.
Preparation example 4
(1) 480g of barium sulfate, 780g of absolute ethyl alcohol, 1.55kg of deionized water and 3g of N-2-aminoethyl-3-aminopropyl trimethoxysilane are weighed, added into a reaction vessel and stirred at 45 ℃ for reaction for 7 hours to form a mixed solution A.
(2) And filtering, washing and drying the mixed solution A to obtain the modified barium sulfate B.
(3) 380g of modified barium sulfate B, 155g of copper nitrate, 28g of reducing agent glucose and 1.5kg of deionized water are weighed and sequentially added into a reaction vessel, the reaction vessel is placed into a microwave reactor, the power of the microwave reactor is 650W, and the reduction reaction is carried out for 7 hours, so that a mixed solution C is obtained.
(4) And (3) performing ultrasonic dispersion on the mixed solution C for 6 hours, separating by using a centrifugal machine, filtering, washing and drying to obtain the modified barium sulfate M4.
Example 4
(1) 100 parts of PP, 9 parts of modified barium sulfate M4, 0.1 part of Irganox1010 and 0.2 part of Irganox1330 are weighed, mixed and stirred uniformly to obtain a mixture;
(2) And (3) extruding and granulating the mixture obtained in the step (1) to obtain the PP composite material P4.
Wherein the temperature and the screw rotating speed of each zone of the double-screw extruder are respectively as follows: the temperature of the first area is 195 ℃, the temperature of the second area is 235 ℃, the temperature of the third area is 235 ℃, the temperature of the fourth area is 235 ℃, the temperature of the fifth area is 235 ℃, the temperature of the sixth area is 235 ℃, the temperature of the machine head is 235 ℃, and the rotating speed of the screw is 255r/min.
Preparation example 5
(1) 460g of barium sulfate, 660g of absolute ethyl alcohol, 1.35kg of deionized water and 2g of N-2-aminoethyl-3-aminopropyl trimethoxysilane are weighed, added into a reaction vessel and stirred for reaction at 55 ℃ for 7 hours to form a mixed solution A.
(2) And filtering, washing and drying the mixed solution A to obtain the modified barium sulfate B.
(3) 320g of modified barium sulfate B, 140g of copper nitrate, 25g of reducing agent glucose and 1.35kg of deionized water are weighed, sequentially added into a reaction vessel, the reaction vessel is placed into a microwave reactor, the power of the microwave reactor is 650W, and the reduction reaction is carried out for 6 hours, so as to obtain a mixed solution C.
(4) And (3) performing ultrasonic dispersion on the mixed solution C for 5 hours, separating by using a centrifugal machine, filtering, washing and drying to obtain the modified barium sulfate M5.
Example 5
(1) 100 parts of PP, 7 parts of modified barium sulfate M5, 0.2 part of Irganox1010 and 0.2 part of Irganox1330 are weighed, mixed and stirred uniformly to obtain a mixture;
(2) And (3) extruding and granulating the mixture obtained in the step (1) to obtain the PP composite material P5.
Wherein the temperature and the screw rotating speed of each zone of the double-screw extruder are respectively as follows: the temperature of the first area is 200 ℃, the temperature of the second area is 225 ℃, the temperature of the third area is 225 ℃, the temperature of the fourth area is 225 ℃, the temperature of the fifth area is 225 ℃, the temperature of the sixth area is 225 ℃, the temperature of the machine head is 225 ℃, and the rotating speed of the screw is 270r/min.
Comparative example 1
(1) 100 parts of PP, 7 parts of barium sulfate, 0.2 part of Irganox1010 and 0.2 part of Irganox1330 are weighed, mixed and stirred uniformly to obtain a mixture;
(2) And (3) extruding and granulating the mixture obtained in the step (1) to obtain the PP composite material D1.
Wherein the temperature and the screw rotating speed of each zone of the double-screw extruder are respectively as follows: the temperature of the first area is 200 ℃, the temperature of the second area is 225 ℃, the temperature of the third area is 225 ℃, the temperature of the fourth area is 225 ℃, the temperature of the fifth area is 225 ℃, the temperature of the sixth area is 225 ℃, the temperature of the machine head is 225 ℃, and the rotating speed of the screw is 270r/min.
The PP composite materials prepared in examples 1 to 5 and comparative example 1 were subjected to performance test, and the test results are shown in Table 1 below.
TABLE 1 Performance test results
As can be seen from the table, the antibacterial property and the high light performance of the examples 1-5 are better than those of the comparative example 1, which shows that the PP composite material of the invention has better antibacterial property and higher glossiness than the common PP material. In addition, the PP composite material prepared by the invention has excellent mechanical properties, and compared with the common PP material, the PP composite material prepared by the invention has higher tensile strength and cantilever beam notch impact strength.
The PP composite material with excellent antibacterial property and high light performance is prepared by the method, the defects of the existing material are overcome, the application field of the PP composite material is greatly expanded, and the method has important significance.
The foregoing disclosure is merely illustrative of some embodiments of the present application and the present application is not limited thereto, as variations may be envisioned by those skilled in the art and are within the scope of the present application.
Claims (5)
1. A highlight antibacterial PP composite material is characterized in that: the highlight antibacterial PP composite material is prepared from the following components in parts by weight:
100 parts of PP (polypropylene) and the total weight of the PP,
6-10 parts of modified barium sulfate,
0.1 to 0.5 part of antioxidant,
the modified barium sulfate is prepared by the following steps:
(1) Dispersing barium sulfate in the dispersion liquid, adding N-2-aminoethyl-3-aminopropyl trimethoxysilane, mixing and stirring to form a mixed liquid A; the dispersion liquid is a mixed liquid of absolute ethyl alcohol and deionized water; the mass ratio of the barium sulfate, the absolute ethyl alcohol, the deionized water and the N-2-aminoethyl-3-aminopropyl trimethoxysilane is (40-50): (60-80): (120-160): (0.1-0.3); the conditions of mixing and stirring are as follows: stirring and reacting for 6-8h at 40-60 ℃;
(2) Filtering the mixed solution A to obtain a solid substance, and washing and drying the solid substance in sequence to obtain modified barium sulfate B;
(3) Mixing modified barium sulfate B, copper salt, reducing agent glucose and deionized water, adding into a reaction vessel, placing the reaction vessel into a microwave reactor, and carrying out reduction reaction for 6-8h to obtain a mixed solution C; the mass ratio of the modified barium sulfate B to the copper salt to the reducing agent glucose to the deionized water is (30-40): (10-16): (1-3): (100-160);
(4) And (3) performing ultrasonic dispersion on the mixed solution C for 4-6 hours, and sequentially performing centrifugal separation, filtration, washing and drying to obtain the modified barium sulfate.
2. The highlight antibacterial PP composite according to claim 1, characterized in that: in the step (3), the copper salt is copper nitrate or copper sulfate; the power of the microwave reactor is 550-750W.
3. The highlight antibacterial PP composite according to claim 1, characterized in that: the antioxidant is at least one of tri (2, 4-di-tert-butyl) phenyl phosphite, tetra [ beta- (3, 5-di-tert-butyl-4-hydroxy phenyl) propionic acid ] pentaerythritol ester and 1,3, 5-trimethyl-2, 4,6- (3, 5-di-tert-butyl-4-hydroxy benzyl) benzene.
4. A method for preparing a highlight antibacterial PP composite material according to any one of claims 1-3, characterized in that: the method comprises the following steps:
(1) Weighing 100 parts of PP, 6-10 parts of modified barium sulfate and 0.1-0.5 part of antioxidant, mixing and stirring uniformly to obtain a mixture;
(2) And (3) extruding and granulating the mixture obtained in the step (1) to obtain the PP composite material.
5. The method for preparing the highlight antibacterial PP composite material according to claim 4, wherein the method comprises the following steps: the step (2) comprises the following steps: putting the mixture obtained in the step (1) into a hopper of a double-screw extruder for extrusion granulation, wherein the double-screw extruder comprises six temperature areas which are sequentially arranged, and the temperatures of the areas are respectively as follows: the temperature of the first area is 180-200 ℃, the temperature of the second area is 220-240 ℃, the temperature of the third area is 220-240 ℃, the temperature of the fourth area is 220-240 ℃, the temperature of the fifth area is 220-240 ℃, and the temperature of the sixth area is 220-240 ℃; the temperature of the head of the double-screw extruder is 220-240 ℃ and the screw rotating speed is 200-280 r/min.
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