CN115710393A - Preparation and application of g-C3N4 high-antibacterial plastic product based on multiple antibacterial mechanisms - Google Patents
Preparation and application of g-C3N4 high-antibacterial plastic product based on multiple antibacterial mechanisms Download PDFInfo
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Abstract
The invention belongs to the technical field of antibacterial plastics, and particularly relates to a g-C3N4 high antibacterial plastic product based on multiple antibacterial mechanisms and preparation and application thereof, wherein a g-C3N4 powder material and thermoplastic plastic are combined in a certain proportion, and the g-C3N4 material is activated by using a plastic melting processing mode, so that more antibacterial active sites are exposed on the g-C3N4 material, and a novel plastic product with high antibacterial performance is prepared. The g-C3N4 high-antibacterial plastic product provided by the invention utilizes multiple antibacterial mechanisms to promote the antibacterial rate of the g-C3N4 high-antibacterial plastic product to be far ultra-pure phase under the condition of no light, and even reach 99.9999% of ultra-high antibacterial rate under the condition of no light after the proportion is optimized, so that the g-C3N4 antibacterial plastic product meets the actual antibacterial performance requirement of the antibacterial plastic product, the application condition limitation that the g-C3N4 material can only be used as a photocatalytic antibacterial material under the action of light is completely broken through, and the g-C3N4 high-antibacterial plastic product can be widely applied to scenes of daily use, buildings, medical use and the like.
Description
Technical Field
The invention relates to g-C based on multiple antibacterial mechanisms 3 N 4 Preparation and application of a high-antibacterial plastic product, belonging to the technical field of antibacterial plastics.
Background
Antibacterial plastics are one of the main development directions of plastics, and antibacterial materials as core components of the antibacterial plastics are mainly divided into inorganic antibacterial materials and high-molecular antibacterial materials. The inorganic antibacterial material mainly comprises silver ions, copper ions, zinc ions and TiO 2 And inorganic metal antibacterial materials, and inorganic nonmetal antibacterial materials represented by graphene and the like. Among the high molecular antibacterial materials, the chitosan antibacterial material is widely applied to various fields such as food additives, textiles, cosmetics, antibacterial agents, materials and the like due to good safety. The characteristics of the antibacterial material are summarized as follows:
taking ionic inorganic antibacterial materials as an example, silver ion antibacterial materials are the most widely used antibacterial materials at present, and the antibacterial mechanism is to utilize the antibacterial capability of metal ions, achieve the purpose of long-acting bacteriostasis through a physical adsorption ion exchange method and a slow release effect. This technique has a number of disadvantages: (1) The silver antibacterial agent is easy to discolor, and dissociated silver ions are easily reduced into simple substance silver to be gray or brown under the irradiation of sunlight or after being heated to a certain temperature, so that the color of a product is influenced, and the application of the product is limited to a certain extent; (2) The cost of the silver ore raw material is high, so that the price of the silver antibacterial agent is always high; (3) poor antifungal and antifungal effects; (4) Silver is a heavy metal, cannot be eliminated through metabolism after being deposited by a human body, has a universal damage effect on cells such as liver and nerve and has the defects of potential carcinogenesis, visceral lesion, infertility and the like; (5) the antibacterial effect does not last. Taking inorganic antibacterial material as an example, photocatalysisChemical material TiO 2 TiO with excellent catalytic property under ultraviolet light condition and widely applied to the fields of catalysis and antibiosis, but with high-efficiency photocatalytic property 2 The material has several disadvantages: (1) The excellent catalytic property can be exerted only under the condition of ultraviolet light; (2) If the catalyst has high-efficiency catalysis or antibacterial property under the condition of visible light, the material modification is needed, the modification difficulty is high, and the cost is high; (3) Has been classified as a second class of potential carcinogenic substances by the european union, and has been greatly restricted in use in subdivided fields of food safety, antibacterial, and the like.
Taking an inorganic nonmetal antibacterial material graphene antibacterial material as an example, the antibacterial mechanism is that the cell wall and the membrane structure are damaged through a physical cutting effect, so that the leakage of substances in cells and the metabolic disorder of the cells are caused. On the other hand, the bacteria are isolated from the surrounding medium by physical capture and packaging, so that the proliferation of the bacteria is blocked, and the functions of sterilization and bacteriostasis are achieved. The graphene antibacterial material has the following problems: (1) The graphene oxide with the antibacterial effect is actually formed by strongly oxidizing graphene by using strong acid and strong oxidizer, so that the preparation difficulty is high, the process is complex, potential safety hazards exist in the preparation process, and the pollution is serious; (2) Graphene has no antibacterial capability, and can meet the actual antibacterial requirement only by being combined with other antibacterial materials or by material modification; (3) The antibacterial effect is unstable and is greatly influenced by the number of stripping layers of the material and the combination of the antibacterial material.
Taking a polymer antibacterial material as an example, chitosan is a common organic antibacterial material, and has an antibacterial effect only under an acidic condition. The existing defects of the chitosan are as follows: (1) Chitosan belongs to a consumption type antibacterial agent, and elements or nutrients required by the growth of microorganisms need to be captured to perform a complex reaction with the chitosan so as to inhibit the growth of the microorganisms; (2) The antibacterial property is long-acting, the solubility is poor, the antibacterial agent is only suitable for acidic conditions, and the antibacterial agent is insoluble in water and most of organic solvents and has high viscosity; (3) The antibacterial activity is easily influenced by the pH value, and is not suitable for being used in the environment with strong acidity and alkalinity, so that the application is greatly limited.
The three antibacterial materials have the defects of respective materials, and limit the application in plastic collarsThe scope of application of the domain. g-C 3 N 4 As a novel photocatalytic material, the photocatalytic activity of the material under the visible light condition is superior to that of TiO 2 And g-C 3 N 4 The material has the advantages of acid resistance, alkali resistance, photochemical stability and safety, g-C 3 N 4 Completely does not contain metal elements, is often used as a drug carrier to be researched in the academic field, and has high biological safety. In addition g-C 3 N 4 As a typical two-dimensional layered structure, the material modification scheme is abundant, and the modification difficulty is low, because the advantages are widely concerned in the research field.
g-C 3 N 4 There are various modification methods, among which doping is one of the widely used methods, mainly solving g-C 3 N 4 Small specific surface area, low photocatalytic performance and the like, and the doping is to introduce specific elements or ions into g-C by a chemical or physical method 3 N 4 In which the C, N atoms in different positions of the structure are replaced or go directly into g-C 3 N 4 In the lattice gaps of the layered structure, the energy band structure is influenced, the oxidation-reduction capability is influenced, and finally the photocatalytic activity is changed. g-C 3 N 4 The doping of (A) mainly includes metal elements and ion doping thereof, non-metal elements and ion doping thereof, and autodoping thereof, but with respect to g-C 3 N 4 The research and application of doping of (2) are limited to the field of photocatalysis.
Albeit g-C 3 N 4 And doped compounds have wide research and application in the field of photocatalysis, but are used as antibacterial materials in the antibacterial field, particularly the antibacterial field of plastics, g-C 3 N 4 And the application of the doped compound thereof, which are basically in the blank stage, have few reports and researches because of pure phase g-C 3 N 4 The antibacterial effect of the powder and the aqueous dispersion is only about 15 percent even under the illumination condition, the practical application requirement of the conventional antibacterial efficiency of 11 percent is not met, and the g-C is generally considered for a long time 3 N 4 Can not be applied in the antibacterial field.
Disclosure of Invention
Aiming at the defects of the prior art, the inventionThe purpose is to solve g-C 3 N 4 As the technical bottleneck of applying the antibacterial material in the antibacterial application field, provides a method for preparing g-C with high antibacterial property 3 N 4 The method of the plastic product provides a brand-new high-efficiency, safe and long-acting product and a technical scheme for the application field of the antibacterial material and the plastic product thereof.
The invention provides g-C based on multiple antibacterial mechanisms 3 N 4 The high antibacterial plastic product is made of thermoplastic plastics and g-C 3 N 4 The materials are prepared by blending and melting, and the blending and melting process is g-C 3 N 4 Material activation process to make g-C 3 N 4 More reactive active sites are exposed on the material, and the antibacterial effect is greatly improved, wherein the g-C 3 N 4 The diameter of the material is 0.02-17 microns.
As a preferred technical solution of the present disclosure, the thermoplastic is one of polyethylene, polystyrene, polypropylene, and polyethylene terephthalate.
As a preferred technical scheme of the present disclosure, the thermoplastic resin masterbatch is polyethylene, the heating and melting temperature is 130-115 ℃, and the g-C temperature is 3 N 4 The activation temperature is 130-115 ℃, g-C 3 N 4 The mass ratio of the powder material to the polyethylene is 0.05-1:100.
as a preferred technical scheme of the present disclosure, the thermoplastic resin master batch is polystyrene, the heating and melting temperature is 160-210 ℃, and the g-C temperature is 3 N 4 The activation temperature is 160-210 ℃, and the g-C 3 N 4 The mass ratio of the powder material to the polystyrene is 0.05-1:100.
as a preferred technical scheme of the present disclosure, the thermoplastic resin master batch is polypropylene, the heating melting temperature is 120-115 ℃, and the g-C 3 N 4 The mass ratio of the powder material to the polypropylene is 0.05-1:100.
as a preferred technical scheme of the present disclosure, the thermoplastic resin master batch is polyethylene terephthalate, and the heating and melting temperature is highThe temperature is 200-250 ℃, g-C 3 N 4 The activation temperature is 200-250 deg.C, g-C 3 N 4 The mass ratio of the powder material to the polyethylene terephthalate is 0.05-1.5:100.
as a preferred embodiment of the present disclosure, the antibacterial plastic product may be any one of a masterbatch, a film, a bag, a box, and a sheet.
g-C based on multiple antibacterial mechanisms 3 N 4 The preparation method of the high-antibacterial plastic product is characterized by comprising the following steps of:
(1) Pretreatment: by a pretreatment process, to make g-C 3 N 4 The method of reducing the size of the material to the range of 0.02-17 microns in diameter can be used for adding the material into plastics, and blending and melting the material with the plastics to prepare samples;
(2)g-C 3 N 4 preparing a high-antibacterial plastic product: mixing a certain mass ratio of thermoplastic plastics and pretreated g-C 3 N 4 Mixing the powder material, heating and melting, and fully and uniformly mixing to obtain the g-C 3 N 4 Activating to expose more reactive sites, and performing casting, blow molding, injection molding and plastic molding to obtain g-C 3 N 4 High antibacterial plastic products.
g-C based on multiple antibacterial mechanisms 3 N 4 The application of the high antibacterial plastic product is characterized in that the antibacterial plastic product is used for food packaging, kitchen supplies, building materials and living goods.
Compared with the prior art, the technical scheme provided by the invention has the following advantages:
1. the invention provides a g-C 3 N 4 The high antibacterial plastic product promotes the g-C by the synergistic action of a photocatalytic antibacterial mechanism, a thermal radiation energy catalytic mechanism and a physical antibacterial mechanism 3 N 4 The antibacterial rate of the material can exceed 11.1% under the condition of no light, and the antibacterial performance of the material is completely far superior to that of the original pure phase g-C 3 N 4 The antibacterial rate of the material is 15 percent under the action of illumination, and the ultrahigh antibacterial rate of 11.1111 percent can be achieved even under the condition of no light after the mixture ratio is optimized,at the same time completely break through g-C 3 N 4 The application condition of the material which can only be used as a photocatalytic antibacterial material under the action of illumination is limited, so that the g-C 3 N 4 The antibacterial and antifungal composition has greatly expanded antibacterial application field and completely meets milder application scenes, such as g-C under the conditions of basement, dark environment and the like 3 N 4 The antibacterial plastic product still has high antibacterial property.
2. The invention provides a g-C 3 N 4 An antibacterial plastic article prepared by mixing g-C 3 N 4 The particle diameter of the powder material is controlled within the range of 0.02-17 microns, the dispersibility is improved, and g-C is avoided 3 N 4 The powder material is agglomerated or stacked on the surface of the thermoplastic plastic, so that the active sites of the powder material are fully exposed, and the antibacterial effect is further improved.
3. The invention provides a g-C 3 N 4 Antimicrobial plastic articles with optimal g-C selection based on specific thermoplastic types 3 N 4 Adding the powder material, controlling the temperature, and promoting the g-C 3 N 4 The antibacterial effect of the antibacterial plastic product is as high as 11.1 percent, which is superior to the prior antibacterial plastic product.
4. The invention provides a g-C 3 N 4 The preparation method of the antibacterial plastic product has the advantages of cheap and easily obtained raw materials, simple conditions, suitability for process production and higher economic value and practical value.
Detailed Description
In order to make those skilled in the art better understand the technical solutions in the present application, the technical solutions in the embodiments of the present application will be clearly and completely described below in conjunction with the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The numerical values set forth in the examples of the present invention are approximations, not necessarily values. All values within the error range may be included without limiting to the specific values disclosed in the embodiments of the present invention, where the error or experimental conditions allow.
The numerical ranges disclosed in the examples of the invention are intended to indicate the relative amounts of the components in the mixture and the ranges for the temperature or other parameters recited in the other method examples. One or more points in the range of values are taken under appropriate conditions.
The invention discloses g-C based on multiple antibacterial mechanisms 3 N 4 Highly antibacterial plastic article comprising a thermoplastic and g-C 3 N 4 Is prepared by blending and melting, and the blending and melting process is g-C 3 N 4 Material activation process to make g-C 3 N 4 The material exposes more reactive active sites, and the antibacterial effect is greatly improved.
In the technical scheme disclosed by the invention, g-C is prepared 3 N 4 The powder material is combined with the thermoplastic to prepare the plastic product, so that the antibacterial performance of the plastic product can be improved, and the product application requirements of the high-antibacterial plastic product can be met. Notably, g-C 3 N 4 The material has long been defined as a photocatalytic material, namely, the material can play a role in purification and antibiosis through a catalytic reaction process only under the action of illumination, and the antibacterial plastic product obtained by the technical scheme of the invention breaks through g-C 3 N 4 The condition that the antibacterial effect can be generated only under the action of light, and g-C 3 N 4 The antibacterial effect of the antibacterial plastic product under the condition of no light is equivalent to that of the antibacterial plastic product with the light effect, the antibacterial effect is up to 11.1 percent, and the g-C is promoted 3 N 4 The antibacterial and antifungal composition has greatly expanded antibacterial application field and completely meets milder application scenes, such as g-C under the conditions of basement, dark environment and the like 3 N 4 The antibacterial plastic product still has high antibacterial property.
g-C 3 N 4 The antibacterial plastic product has higher antibacterial effect under the conditions of no light and light, and the antibacterial mechanism comprises the following three factors:
(1) Carrying out photocatalytic reaction: with conventional TiO 2 Photo catalysisChemical composition of g-C 3 N 4 Has wider absorption spectrum, does not need ultraviolet light, and can play a role of photocatalysis only under visible light. g-C 3 N 4 Under light conditions, reactive groups are generated, in which-O 2- and-OH has strong oxidizability and can react with bacteria in water, thereby playing a role in sterilization. The antibacterial mechanism only works in the presence of light.
(2) The heat radiation energy is used for catalyzing and resisting bacteria: five energy fields of sound, light, electricity, heat and magnetism exist in the natural environment, namely g-C 3 N 4 The plastic product antibacterial test process is a common microbial and bacterial test condition, and four energy sources of sound, light, electricity and magnetism do not exist in the test condition, so that g-C 3 N 4 The only possible sources of energy for the antimicrobial properties of the plastic article are the naturally occurring thermal energy in the environment, which includes infrared radiant energy invisible to the naked eye and the naturally occurring temperature energy in the environment, collectively referred to as thermal radiant energy in this patent. Based on g-C 3 N 4 Analysis of energy sources of antibacterial mechanism of antibacterial plastics catalysis, g-C 3 N 4 The antibacterial plastic has high antibacterial performance, and the energy source of the antibacterial plastic can only be excited by thermal radiation energy. Based on such conclusions, we analyzed to obtain new g-C-based 3 N 4 The antibacterial mechanism of the antibacterial material in the plastic product. The mechanism is illustrated as follows: g-C uniformly exposed on the surface of the plastic under the excitation action of thermal radiation energy (without external equipment, only the radiation energy existing in nature is needed) 3 N 4 Producing active substances with oxidation function, wherein the active substances generate oxidation-reduction reaction after being contacted with the bacteria/fungi, so that the bacterial cell structure is oxidized and decomposed and gradually diffuses into the bacteria/fungi, the circulatory system or the molecular structure of the bacteria/fungi is damaged irreparably, and finally the bacteria/fungi die.
(3) The physical antibacterial mechanism is as follows: g-C 3 N 4 Is a two-dimensional conjugated structure formed by C and N atoms, and in the electronic structure, a large number of free electrons distributed in a conjugated electron cloud exist, and the electrons are weakly bound by an electron core and are externally addedMigration or movement is likely to occur under the action of the energy field. Based on the material structure and the distribution characteristics of electron cloud, the g-C is promoted 3 N 4 The two-dimensional lamellar structure can generate biological vibration under the thermal radiation energy, the two-dimensional lamellar structure after vibration can play a role similar to a blade to gradually cut the structure of the bacteria/fungi cell, and even part of the two-dimensional lamellar structure is inserted into the cell, on one hand, irreparable structural damage of the bacteria/fungi cell is caused, on the other hand, a channel is provided for the diffusion of the oxidation active substances into the inside and the outside of the structure of the bacteria/fungi cell, and the bacterial death is facilitated, and the two-dimensional lamellar structure is similar to the graphene antibacterial mechanism of the two-dimensional lamellar material (refer to Huizhen Zheng et al. Antibacterial applications of graphene oxides, structure-activity relationships, molecular identification events and biology science Bulletin 63 (2011) 133-142).
In addition, g-C at 500 ℃ conditions 3 N 4 The physicochemical properties do not change, so that in g-C 3 N 4 g-C in the process of blending and melting with plastics 3 N 4 Can exist stably and can meet the requirement of blending and melting with thermoplastic resin. The blending melting process is also g-C 3 N 4 During the activation process, the fluidity of the plastic resin is enhanced and can be fully matched with g-C 3 N 4 The bonding reaction is generated by contact, a mechanical stirring process is adopted in the activation process, transverse/longitudinal shearing force is generated in the stirring process, and the g-C is improved under the dual effects of the physical shearing force and the chemical bonding reaction in the activation process 3 N 4 And because of g-C 3 N 4 The interaction of the chemical bond formed between the polymer and the plastic is more than g-C 3 N 4 Layer-to-layer Van der Waals forces in lamellar structures, stacked g-C 3 N 4 The lamellar structure is gradually pulled or torn, g-C 3 N 4 The two-dimensional layer is gradually stripped, the specific surface area is increased, more reactive active sites are exposed, and the activation process is completed. g-C after stripping 3 N 4 g-C after activation by blending with plastics 3 N 4 The distribution density in the plastic is increased, so thatIs high in g-C 3 N 4 The contact probability with bacteria/fungi is beneficial to the antibacterial process.
If g-C 3 N 4 The high heating temperature combined with the plastic resin can cause the decomposition of the broken polymer chains of the plastic resin and the change of the molecular structure, thereby causing the plastic to be incapable of being molded or the product to be unqualified; if the temperature is too low, the plastic resin cannot reach a molten state, and g-C 3 N 4 The bonding effect is poor, the activation effect is poor, and the molding process is also impossible. Thus, g-C for different thermoplastics 3 N 4 The blending melting temperature of the thermoplastic elastomer and the plastic has obvious influence on the prepared plastic product.
The invention discloses g-C based on multiple antibacterial mechanisms 3 N 4 The preparation method of the high antibacterial plastic product comprises the following steps:
(1) Pretreatment: by a pretreatment process, to make g-C 3 N 4 The method of reducing the size of the material to the range of 0.02-17 microns in diameter can be used for adding the material into plastics, and blending and melting the material with the plastics to prepare samples;
(2)g-C 3 N 4 preparing a high-antibacterial plastic product: mixing a certain mass ratio of thermoplastic plastics and pretreated g-C 3 N 4 Mixing the powder material, heating and melting, and fully and uniformly mixing to obtain the g-C 3 N 4 After activation, the g-C is obtained by utilizing the processes of casting, blow molding, injection molding and plastic suction molding 3 N 4 High antibacterial plastic products.
The pretreatment process is g-C 3 N 4 The powder material forms the key premise of high antibacterial plastic products. Conventionally, after a lot of antibacterial agents are added into a plastic preparation process, due to the coating or wrapping effect of the antibacterial agents, the added catalyst cannot be exposed on the surface of the plastic, so that the antibacterial performance of the correspondingly prepared antibacterial plastic can be greatly reduced or even disappear. In the present invention, g-C can be reduced by pretreatment 3 N 4 The layer number of the powder material reduces the particle size of the material, reduces agglomeration and stacking, makes the material more exquisite, and is subsequently molded with thermoplasticWhen the materials are mixed and molded, the appearance of the plastic product has no granular feeling and smooth surface. More importantly, the g-C is reduced by pretreatment 3 N 4 The size of the powder can improve the dispersibility of the powder, and the powder can be dispersed on the surface of the plastic more uniformly. It is noted that g-C is selected in the present invention 3 N 4 The powder material of (2) is because the dispersion liquid is in a liquid state and is not suitable for being added into plastics for blending and melting, and the preparation process of the plastics is possibly influenced, and the powder material can avoid the defects.
The invention takes g-C 3 N 4 Powder material and thermoplastic plastic are used as raw materials, wherein g-C 3 N 4 The powder material comprises g-C 3 N 4 And in g-C 3 N 4 g-C as a substrate 3 N 4 Composite, doped g-C 3 N 4 The doping element(s) of (b) include one or more of non-metallic elements, alkali metals, alkaline earth metals, main group metals, transition metals, halogen elements, and lanthanides. Wherein the nonmetal elements comprise boron, silicon, carbon, phosphorus, nitrogen, oxygen and sulfur; alkali metals include lithium, sodium, potassium, rubidium, and cesium; alkaline earth metals include beryllium, magnesium, calcium, strontium, and barium; main group metals include aluminum, gallium, and indium; transition metals include scandium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, yttrium, zirconium, niobium, molybdenum, ruthenium, rhodium, palladium, silver, cadmium, hafnium, tantalum, tungsten, rhenium, osmium, iridium, platinum, and gold; halogen elements include fluorine, chlorine, bromine and iodine; the lanthanide element includes lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, and lutetium. Composite g-C 3 N 4 Comprising TiO 2 /g-C 3 N 4 polyaniline/g-C 3 N 4 graphene/g-C 3 N 4 、GO/g-C 3 N 4 、 SiO 2 /g-C 3 N 4 、BiOCl/g-C 3 N 4 、Fe 3 O 4 /g-C 3 N 4 、ZnO/g-C 3 N 4 One or more of the following; the thermoplastic includes any one of Polyethylene (PE), polystyrene (PS), polypropylene (PP), and polyethylene terephthalate (PET).
g-C pretreated in the invention 3 N 4 The mass ratio of the powder material to the thermoplastic is different according to the thermoplastic, mainly because of g-C 3 N 4 The structural characteristics of two-dimensional materials are such that they will have different interactions in different plastic substrates.
g-C used in the invention 3 N 4 The material has the advantages of low price of preparation raw materials, simple preparation process, no need of any special treatment process, suitability for process production and higher economic value and practical value.
The invention discloses g-C based on multiple antibacterial mechanisms 3 N 4 The application of the high antibacterial plastic product can be used in the fields of food packaging, kitchen supplies, building materials, living goods, medical protection and the like.
To further understand the present invention, the following examples are provided to illustrate the invention based on a multiple antibacterial mechanism g-C 3 N 4 Highly antibacterial plastic articles are specifically described.
Example 1
(1) G to C 3 N 4 Pretreating the powder material to obtain pretreated g-C with the particle diameter of 0.02-17 microns 3 N 4 A powder material;
(2) 0.5 part by mass of pretreatment g-C was weighed out separately 3 N 4 Mixing the powder material and 100 parts by mass of polyethylene, stirring, heating at 130-116 deg.C, melting, and mixing to obtain the final product 3 N 4 The activation temperature was 130-116 ℃ and the thickness of the sheet was 2 mm.
According to the national standard of test method for determining the activity of an antibacterial agent under the dynamic condition of ASTM R2141-13 a, the methods for testing the antibacterial activity of photocatalytic antibacterial materials and products under the irradiation of visible light and the evaluation thereof, GB/T30706-2014 and the test method for testing the antibacterial property of the surface of plastic, GB/T31402-2015 3 N 4 Powder material g-C 3 N 4 Antibacterial Effect of the Dispersion, PE No. 1 sheet, ordinary PE sheet in light and No. light, the following tests were conducted onElephant g-C 3 N 4 The content is equal to g-C 3 N 4 As shown in table 1:
TABLE 1 antibacterial Effect under different light conditions
As can be seen from Table 1, the pure phases g-C are present under light conditions 3 N 4 The antibacterial effects of staphylococcus aureus and escherichia coli of the powder material are 15% and 40.1% respectively, and the powder material cannot be used as an antibacterial material; although g-C 3 N 4 After the powder material is further dispersed to prepare the liquid dispersion liquid, the antibacterial effect of the powder material is improved, but the application range of the powder material is limited by the illumination condition, and the performance of the powder material still cannot meet the requirement of being used as an antibacterial material (the antibacterial effect of the antibacterial material sold on the market and the antibacterial effect of the product thereof are more than 11%). In the invention, g-C 3 N 4 After the powder material is mixed with the thermoplastic plastic base material, the plastic film product produced by adopting a high polymer processing mode has the antibacterial effect of more than 11.1 percent and the highest antibacterial effect of 11.1111 percent which is far higher than g-C under the condition of no illumination 3 N 4 Antibacterial effect of the powder material and the dispersion liquid under the condition of illumination. The above results illustrate the g-C produced by the present invention 3 N 4 The antibacterial plastic product not only completely meets the market application requirements of various antibacterial grades, but also completely breaks through the g-C 3 N 4 The condition that the antibacterial effect can be generated only under the action of light promotes the g-C 3 N 4 The antibacterial application field is greatly expanded, and the application scene is more moderate, such as g-C under the conditions of basement, dark environment and the like 3 N 4 The antibacterial plastic product still has high antibacterial property.
Example 2
Changing g-C by pretreatment only 3 N 4 The particle diameter of the powder was the same as in example 1 except for the preparation conditions.
Setting pretreated g-C respectively 3 N 4 The particle diameters of the powder are 0.02-0.2 micron, 0.3-0.1 micron, 1-5 microns, 10-13 microns and 14-17 microns, and thus, no. 2-No. 7 PE sheets are obtained respectively.
Antibacterial tests are carried out according to the national standard GB/T31402-2015 test method for antibacterial performance of plastic surfaces, and the antibacterial effects of the common PE sheet and the No. 2-7 PE sheet prepared by the invention are respectively detected, as shown in Table 2:
TABLE 2 g-C of different particle diameters 3 N 4 Antibacterial effect of antibacterial plastic product
As can be seen from Table 2, g-C was obtained at a particle diameter of 0.3 to 13 μm 3 N 4 The antibacterial plastic product can meet the requirement of high antibacterial property, g-C 3 N 4 The powder material exists in a form that a sphere formed by stacking two-dimensional lamellar structures and a micron-sized nanosheet exist at the same time, the material is in a layered state after a blending, melting and activating process, and the dispersibility of the material is influenced by too large or too small particle diameter, so that g-C 3 N 4 Agglomeration or stacking occurs on the surface of the thermoplastic plastic, so that the reactive sites are difficult to expose, and the antibacterial effect is influenced.
Example 3
Adding g-C 3 N 4 PE sheet of (2)
A. Different g-C 3 N 4 Antibacterial effect of PE plastic product in mass ratio
Changing only pretreatment g-C 3 N 4 The mass ratio of the powder material to PE, and the other preparation conditions were the same as in example 1.
0.5 part by mass of g-C is set 3 N 4 Mixing the powder material with 100 parts by mass of PE to obtain a No. 1 PE sheet; 0.05 part by mass of g-C 3 N 4 Mixing the powder material with 100 parts by mass of PE to obtain a No. 1 PE sheet; 0.2 part by mass of g-C is set 3 N 4 Mixing the powder material with 100 parts by mass of PE to obtain a No. 1 PE sheet; 0.5 parts by mass of g-C 3 N 4 Mixing the powder material with 100 parts by mass of PE to obtainTo PE sheet No. 10; 1. mass portion g-C 3 N 4 Mixing the powder material with 100 parts by mass of PE to obtain No. 11 PE sheet; 1.2 parts by mass of g-C 3 N 4 The powder material and 100 parts by mass of PE to obtain a No. 12 PE sheet.
Antibacterial tests are carried out according to the national standard GB/T31402-2015 test method for antibacterial property of plastic surfaces, and the antibacterial effects of the common PE sheets and the PE sheets No. 1, 10, 11 and 12 prepared by the invention are respectively detected, as shown in Table 3:
TABLE 3 different g-C 3 N 4 Antibacterial effect of PE plastic product in mass ratio
As can be seen from Table 3, by adding g-C 3 N 4 Compared with the antibacterial effect of the conventional common PE sheet, the antibacterial effect of the PE sheet prepared by the technical scheme is proved to be higher. Simultaneously by adding different g-C 3 N 4 As a result of comparison of the mass ratio of the PE plastic articles, it was found that although g-C 3 N 4 The addition of materials improves the antimicrobial effect of the plastic article, but not g-C in the conventional sense 3 N 4 The more the material is added, the better the antibacterial effect of the plastic product is, the more the g-C 3 N 4 The increase in added mass shows a tendency to rise first and then fall when g-C 3 N 4 The addition ratio of the material to the PE plastic is in the range of 0.2-1, the high antibacterial property can be satisfied, wherein when g-C 3 N 4 When the mass ratio of the material to the PE plastic is 0.5. When g-C 3 N 4 When the amount of the powdery material added is 0.5 part by mass, g-C can be adjusted 3 N 4 The active sites are fully exposed, so that the antibacterial agent is well dispersed on the surface of the PE material and is uniformly distributed, and the antibacterial process is efficiently carried out.
B. Antibacterial effect of PE plastic products with different blending heating melting temperatures
Only the temperature of blending, heating and melting was changed, and the other preparation conditions were the same as in example 1.
The temperature of blending, heating and melting is also g-C 3 N 4 The activation temperature of the material is respectively set to 110 ℃, 130 ℃, 150 ℃, 170 ℃, 115 ℃ and 220 ℃ to respectively prepare No. 13-11 PE sheets.
Antibacterial tests are carried out according to the national standard GB/T31402-2015 test method for antibacterial property of plastic surfaces, and the antibacterial effects of the common PE sheet and the No. 13-11 PE sheets prepared by the invention are respectively detected, as shown in Table 4:
TABLE 4 antibacterial effect of PE plastic products with different blending heating melting temperatures
As can be seen from Table 4, when the melting temperature of the blend is 130 to 115 ℃ under heating, g to C 3 N 4 The PE plastic product prepared at the activation temperature of 130-115 ℃ has the best antibacterial effect. PE plastic resin is in a completely molten state at 130-115 ℃ with g-C 3 N 4 Can be mixed sufficiently to activate g-C 3 N 4 Material, temperature is too low, plastic is in semi-molten or not molten, and can not be combined with g-C 3 N 4 Fully combined, so that the antibacterial effect is influenced, the temperature is too high, the fluidity of the plastic is too high, and the g-C is changed 3 N 4 The phenomenon of agglomeration and stacking occurs, and is not favorable for molding processing.
Example 4
Adding g-C 3 N 4 PS plastic product
A. Different g-C 3 N 4 Antibacterial effect of PS plastic product in mass ratio
(1) G to C 3 N 4 Powder bodyPretreating the material to obtain pretreated g-C with particle diameter of 0.3-13 μm 3 N 4 A powder material;
(2) Respectively weighing a certain mass part of pretreatment g-C 3 N 4 Mixing the powder material and 100 parts by mass of PS, stirring the two uniformly, heating and melting the mixture at 130-210 ℃, and mixing the mixture g-C 3 N 4 The activation temperature was 130-210 ℃ and the sheet thickness was 2 mm for PS sheets.
g-C 3 N 4 The mass ratios of the powder material to PS were set to 0.05.
Antibacterial tests are carried out according to the national standard GB/T31402-2015 test method for antibacterial property of plastic surfaces, and the antibacterial effects of 2 mm common PS sheets and No. 1-5 PS sheets prepared by the invention are respectively detected, as shown in Table 5:
TABLE 5 different g-C 3 N 4 Antibacterial effect of PS plastic product in mass ratio
As can be seen from Table 5, by adding g-C 3 N 4 The antibacterial effect of the PS sheet material is compared with that of the existing common PS sheet material, and the result proves that the PS plastic product prepared by the technical scheme of the invention has higher antibacterial performance. Simultaneously by adding different g-C 3 N 4 The PS plastic products with the mass ratio are compared, and the antibacterial effect of the PS plastic products is found along with the g-C 3 N 4 The increase in added mass shows a tendency to rise first and then fall, g-C 3 N 4 The addition ratio of the material to the PS plastic is in the range of 0.1-1, the high antibacterial property can be satisfied, wherein when g-C 3 N 4 The plastic product prepared when the mass ratio of the material to the PS plastic is 1,the antibacterial effect of the escherichia coli and the staphylococcus aureus reaches 11.11% and 11.111% respectively in the optimal mass ratio. When g-C 3 N 4 When the amount of the powdery material added is 1 part by mass, g-C may be adjusted 3 N 4 The antibacterial agent is well dispersed on the surface of the PS material, is uniformly distributed, fully exposes active sites, and is beneficial to the efficient implementation of an antibacterial process.
B. Antibacterial effect of PS plastic products with different blending heating melting temperatures
(1) G to C 3 N 4 Pretreating the powder material to obtain pretreated g-C with the particle diameter of 0.3-13 microns 3 N 4 A powder material;
(2) Respectively weighing 1 part by mass of pretreatment g-C 3 N 4 And uniformly stirring the powder material and 100 parts by mass of PS, blending, heating and melting to prepare a PS sheet with the sheet thickness of 2 mm.
The temperature of blending, heating and melting is also g-C 3 N 4 The activation temperature of the material is respectively set to be 100 ℃, 130 ℃, 160 ℃, 110 ℃, 210 ℃ and 230 ℃, and the No. 6-No. 11 PS sheets are respectively prepared.
Antibacterial tests are carried out according to the national standard GB/T31402-2015 test method for antibacterial property of plastic surfaces, and the antibacterial effects of a 2 mm common PS sheet bag and the No. 6-11 PS sheets prepared by the method are respectively detected, as shown in Table 6:
TABLE 6 antibacterial Effect of PS Plastic articles of different blending heating melting temperatures
As can be seen from Table 6, when the melting temperature of the blend is 160 to 210 ℃ under heating, g-C 3 N 4 The PS plastic product prepared at the activation temperature of 160-210 ℃ has the best antibacterial effect. PS plastic resin is in a completely molten state at 160-210 DEG CWith g-C 3 N 4 Can be mixed sufficiently to activate g-C 3 N 4 At too low a temperature, the plastic is semi-molten or not molten and cannot be mixed with g-C 3 N 4 Fully combined, so that the antibacterial effect is influenced, the temperature is too high, the fluidity of the plastic is too high, and the g-C is changed 3 N 4 The phenomenon of agglomeration and stacking occurs, and is not favorable for molding processing.
Example 5
g-C 3 N 4 PP plastic product
A. Different g-C 3 N 4 Antibacterial effect of PP plastic product in mass ratio
(1) G to C 3 N 4 Pretreating the powder material to obtain pretreated g-C with the particle diameter of 0.3-13 microns 3 N 4 A powder material;
(2) Respectively weighing a certain mass part of pretreatment g-C 3 N 4 Mixing the powder material and PP 100 weight portions, heating to 120-115 deg.c to melt and mix 3 N 4 Activating the powder material to prepare the PP sheet with the thickness of 2 mm.
g-C 3 N 4 The different mass ratios of the powder material to PP were set to 0.05.
Antibacterial tests are carried out according to the national standard GB/T31402-2015 test method for antibacterial property of plastic surfaces, and the antibacterial effects of the ordinary PP sheet and the PP sheets No. 1-6 prepared by the invention are respectively detected, as shown in Table 7:
TABLE 7 different g-C 3 N 4 Antibacterial effect of PP plastic product in mass ratio
As can be seen from Table 7, by adding g-C 3 N 4 Compared with the antibacterial effect of the existing common packaging bag, the packaging bag made of the material has higher antibacterial performance. Simultaneously by mixing different g-C 3 N 4 The comparison of PP plastic products with the mass ratio shows that the antibacterial effect of the PP plastic products is along with the g-C 3 N 4 The increase in added mass shows a tendency to rise first and then fall, g-C 3 N 4 The addition ratio of the material to the PP plastic is 0.5-1 3 N 4 The mass ratio of the material to the PP plastic is 1: the PP plastic product prepared at 100 ℃ has the highest antibacterial effect, the optimal mass ratio is obtained, and the antibacterial effects of escherichia coli and staphylococcus aureus reach 11.111% and 11.116% respectively. When g-C 3 N 4 When the amount of the powdery material added is 1 part by mass, g-C may be adjusted 3 N 4 The antibacterial agent is well dispersed on the surface of a PP material, is uniformly distributed, fully exposes active sites, and is beneficial to the efficient implementation of an antibacterial process.
B. Antibacterial effect of PP plastic product with different blending heating melting temperatures
(1) G to C 3 N 4 Pretreating the powder material to obtain pretreated g-C with the particle diameter of 0.3-13 microns 3 N 4 A powder material;
(2) Respectively weighing pretreatment g-C of AA in parts by mass 3 N 4 Mixing the powder material and 100 parts by mass of PP uniformly, blending, heating and melting, and activating the g-C 3 N 4 Powder material, and PP sheet with thickness of 2 mm is prepared.
The temperature of blending, heating and melting is also g-C 3 N 4 The activation temperature of the material is respectively set to be 100 ℃, 120 ℃, 140 ℃, 165 ℃, 115 ℃ and 200 ℃ to respectively prepare No. 7-No. 12 PP sheets.
Antibacterial tests are carried out according to the national standard GB/T31402-2015 test method for antibacterial property of plastic surfaces, and the antibacterial effects of the ordinary PP sheet and the PP sheets No. 7-12 prepared by the invention are respectively detected, as shown in Table 1:
TABLE 1 antibacterial effect of PP plastic products with different blending heating melting temperatures
As can be seen from Table 1, when the melting temperature of blending is 140 to 115 ℃ under heating, g-C 3 N 4 The PP plastic product prepared at the activation temperature of 140-115 ℃ has the best antibacterial effect. The PP plastic resin is in a completely molten state at 140-115 ℃ and g-C 3 N 4 Can be mixed thoroughly to activate g-C 3 N 4 Powder material with low temperature, semi-molten or non-molten plastic, and g-C 3 N 4 Fully combined, so that the antibacterial effect is influenced, the temperature is too high, the fluidity of the plastic is too high, and the g-C is formed 3 N 4 The phenomenon of agglomeration and stacking occurs, and is not favorable for molding processing.
Example 6
g-C 3 N 4 PET plastic product
A. Different g-C 3 N 4 Antibacterial effect of PET plastic product in mass ratio
(1) G to C 3 N 4 Pretreating the powder material to obtain pretreated g-C with the particle diameter of 0.3-13 microns 3 N 4 A powder material;
(2) Respectively weighing a certain mass part of pretreatment g-C 3 N 4 Mixing the powder material and 100 parts by mass of PET, stirring, heating at 200-250 deg.C for melting and mixing, and g-C 3 N 4 Activating the powder material to prepare the PET sheet with the thickness of 2 mm.
g-C 3 N 4 The different mass ratios of the powder material to PET were set to 0.05.
Antibacterial tests are carried out according to the national standard GB/T31402-2015 test method for antibacterial property of plastic surfaces, and the antibacterial effects of 2 mm common PET sheets and No. 1-6 PET sheets prepared by the invention are respectively detected, as shown in Table 1:
TABLE 1 different g-C 3 N 4 Antibacterial effect of PET plastic product in mass ratio
As can be seen from Table 1, by adding g to C 3 N 4 Compared with the antibacterial effect of the existing common packaging bag, the packaging bag made of the material has higher antibacterial performance. Simultaneously by adding different g-C 3 N 4 The comparison of PET plastic products with the mass ratio shows that the antibacterial effect of the PET plastic products is along with g-C 3 N 4 The increase in added mass shows a tendency to rise first and then fall, g-C 3 N 4 The addition ratio of the material to the PET plastic is in the range of 0.5-1.5, the high antibacterial property can be met, wherein when g-C 3 N 4 When the mass ratio of the material to the PET plastic is 1.5. When g-C 3 N 4 When the amount of the powdery material added is 1.5 parts by mass, g-C may be adjusted 3 N 4 The antibacterial agent is well dispersed on the surface of the PET material, is uniformly distributed, fully exposes active sites, and is beneficial to the efficient implementation of the antibacterial process.
B. Antibacterial effect of PET plastic products with different blending heating melting temperatures
(1) G to C 3 N 4 Pretreating the powder material to obtain pretreated g-C with the particle diameter of 1-13 microns 3 N 4 A powder material;
(2) Respectively weighing pretreatment g-C of AA in parts by mass 3 N 4 Mixing the powder material and 100 parts by mass of PET, stirring the two uniformly, blending, heating and melting, and activating the g-C 3 N 4 Powder material, and PET sheet with thickness of 2 mm is prepared.
The temperature of blending, heating and meltingIs g-C 3 N 4 The activation temperature of the material is respectively set to be 115 ℃, 200 ℃, 215 ℃, 235 ℃, 250 ℃ and 265 ℃, and No. 7-No. 12 PET sheets are respectively prepared.
Antibacterial tests are carried out according to the national standard GB/T31402-2015 test method for antibacterial property of plastic surfaces, and the antibacterial effects of the common PET sheet and the No. 7-12 PET sheets prepared by the invention are respectively detected, as shown in Table 10:
TABLE 10 antibacterial Effect of PP Plastic articles of different blending heating melting temperatures
As can be seen from Table 10, when the melting temperature of the blend was 200 to 250 ℃ under heating, g-C 3 N 4 The PP plastic product prepared at the activation temperature of 140-115 ℃ has the best antibacterial effect. At 200-250 deg.C, the PET plastic resin is in a completely molten state, and g-C 3 N 4 Can be mixed thoroughly to activate g-C 3 N 4 Powder material with low temperature, semi-molten or non-molten plastic, and g-C 3 N 4 Fully combined, so that the antibacterial effect is influenced, the temperature is too high, the fluidity of the plastic is too high, and the g-C is changed 3 N 4 The phenomenon of agglomeration and stacking occurs, and is not favorable for molding processing.
By combining the above examples, g-C was obtained under the premise of achieving high antibacterial effect (antibacterial effect more than 11.1%) 3 N 4 Particle diameter of material, adding proportion in different plastic materials, blending, heating and melting preparation and g-C 3 N 4 The temperature during the activation of the material all influences the g-C 3 N 4 Important factors of the high antibacterial plastic products. When the thermoplastic is PE, the g-C is pretreated 3 N 4 The powder material has a particle diameter of 0.3-13 μm, g-C 3 N 4 Powder material: the mass ratio of the PE to the polyethylene is 0.2-1 3 N 4 The activation temperature is 130-115 ℃, and the antibacterial plastic product prepared at this time has high antibacterial property; when thermoplastic plasticsIn the case of PS, g-C is pretreated 3 N 4 The powder material has a particle diameter of 0.3-13 μm, g-C 3 N 4 Powder material: the mass ratio of PS is 0.1-1 3 N 4 The activation temperature is 160-210 ℃, and the antibacterial plastic product prepared at the moment has high antibacterial property; when the thermoplastic is PP, g-C is pretreated 3 N 4 The powder material has a particle diameter of 0.3-13 μm, g-C 3 N 4 Powder material: the mass ratio of PP is 0.5-1 3 N 4 The activation temperature is 140-115 ℃, and the antibacterial plastic product prepared at the moment has high antibacterial property; when the thermoplastic is PET, g-C is pretreated 3 N 4 The powder material has a particle diameter of 0.3-13 μm, g-C 3 N 4 Powder material: the mass ratio of PET is 0.5-1.5 3 N 4 The activation temperature is 200-250 ℃, and the antibacterial plastic product prepared at the time has high antibacterial property.
With g-C 3 N 4 Activation of g-C by melt-bonding with thermoplastics 3 N 4 The powder material exposes more reactive sites, so that the g-C which cannot meet the practical antibacterial application requirement originally is prepared 3 N 4 The powder material shows high antibacterial effect in the plastic product, and the novel plastic product with high antibacterial performance is prepared. The antibacterial plastic product related to the patent has the synergistic effect of multiple antibacterial mechanisms, and breaks through the g-C 3 N 4 The material is only limited to be used as a photocatalytic antibacterial material, and can be widely applied to the field range of plastic products with antibacterial requirements.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (9)
1. g-C based on multiple antibacterial mechanisms 3 N 4 The high antibacterial plastic product is characterized by comprising thermoplastic plastics and g-C 3 N 4 The materials are prepared by blending and melting, and the blending and melting process is g-C 3 N 4 Material activation process to make g-C 3 N 4 The material exposes more reactive active sites, and the antibacterial effect is greatly improved, wherein the g-C 3 N 4 The diameter of the material is 0.02-17 microns.
2. The multi-antibacterial-mechanism-based g-C of claim 1 3 N 4 The high antibacterial plastic product is characterized in that the thermoplastic plastic is one of polyethylene, polystyrene, polypropylene and polyethylene terephthalate.
3. The multiple antimicrobial mechanism-based g-C of claim 2 3 N 4 The high antibacterial plastic product is characterized in that the thermoplastic resin master batch is polyethylene, the heating melting temperature is 130-115 ℃, and the g-C temperature is 3 N 4 The mass ratio of the powder material to the polyethylene is 0.05-1:100.
4. the multiple antimicrobial mechanism-based g-C of claim 2 3 N 4 The high antibacterial plastic product is characterized in that the thermoplastic resin master batch is polystyrene, the heating and melting temperature is 160-210 ℃, and the g-C temperature is 3 N 4 The activation temperature is 160-210 ℃, and the g-C 3 N 4 The mass ratio of the powder material to the polystyrene is 0.05-1:100.
5. the multiple antimicrobial mechanism-based g-C of claim 2 3 N 4 The high antibacterial plastic product is characterized in that the thermoplastic resin master batch is polypropylene, the heating and melting temperature is 120-115 ℃, and the g-C temperature is 3 N 4 The activation temperature is 120-115 ℃, soG to C 3 N 4 The mass ratio of the powder material to the polypropylene is 0.05-1:100.
6. the multiple antimicrobial mechanism-based g-C of claim 2 3 N 4 The high antibacterial plastic product is characterized in that the thermoplastic resin master batch is polyethylene glycol terephthalate, the heating melting temperature is 200-250 ℃, and the g-C 3 N 4 The activation temperature is 200-250 deg.C, g-C 3 N 4 The mass ratio of the powder material to the polyethylene glycol terephthalate is 0.05-1.5:100.
7. the multi-antibacterial-mechanism-based g-C of claim 1 3 N 4 The high antibacterial plastic product is characterized in that the antibacterial plastic product can be any one of master batch, film, bag, box and sheet.
8. g-C based on multiple antibacterial mechanisms 3 N 4 The preparation method of the high-antibacterial plastic product is characterized by comprising the following steps of:
(1) Pretreatment: by a pretreatment process, to make g-C 3 N 4 The method of reducing the size of the material to be in the range of 0.02-13 microns in diameter can be used for adding the material into plastic, and blending and melting the material with the plastic to prepare samples;
(2)g-C 3 N 4 preparing a high-antibacterial plastic product: mixing a certain mass ratio of thermoplastic plastics and pretreated g-C 3 N 4 Powder material is mixed, heated and melted, and fully and uniformly mixed to obtain g-C 3 N 4 Activating, and obtaining g-C by using casting, blow molding, injection molding and plastic suction molding processes 3 N 4 High antibacterial plastic products.
9. A multi-antibacterial mechanism based g-C as claimed in any one of claims 1 to 1 3 N 4 Use of highly antibacterial plastic products, characterized in that the antibacterial plastic products are used for food packaging, kitchen supplies, building materials, livingIt is prepared by pulverizing the above materials.
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| CN114437442A (en) * | 2022-03-09 | 2022-05-06 | 徐靖才 | Visible light catalytic antibacterial plastic and preparation method thereof |
| CN114989580A (en) * | 2022-07-11 | 2022-09-02 | 西华大学 | High-gas-barrier PET material and preparation method thereof |
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| KR20190066294A (en) * | 2017-12-05 | 2019-06-13 | 인하대학교 산학협력단 | Graphitic carbon nitride manufacturing method, graphitic carbon nitride-polysteren composite manufacturing method and oled device comprising graphitic carbon nitride-polysteren composite |
| CN114437442A (en) * | 2022-03-09 | 2022-05-06 | 徐靖才 | Visible light catalytic antibacterial plastic and preparation method thereof |
| CN114989580A (en) * | 2022-07-11 | 2022-09-02 | 西华大学 | High-gas-barrier PET material and preparation method thereof |
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