CN110003630B - Transparent wear-resistant flame-retardant antibacterial plastic and preparation method thereof - Google Patents
Transparent wear-resistant flame-retardant antibacterial plastic and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of modification of thermoplastic high polymer materials, in particular to a transparent wear-resistant flame-retardant antibacterial plastic and a preparation method thereof, wherein the plastic comprises the following components in parts by weight: 100 parts of PC resin, 0.03-0.12 part of sulfonate flame retardant, 0.2-2 parts of silane flame retardant, 0.1-0.5 part of antioxidant, 0.05-0.5 part of lubricant, 0.1-1 part of antibacterial agent and 0.75-3 parts of scratch-resistant agent, and the flame-retardant and antibacterial coating is prepared by mainly drying, mixing, extruding and granulating the components, has good flame retardance, outstanding wear resistance and antibacterial property and good impact property, and is suitable for plastic products which are in close contact with human skin.
Description
Technical Field
The invention relates to the technical field of modification of thermoplastic high polymer materials, in particular to a transparent wear-resistant flame-retardant antibacterial plastic and a preparation method thereof.
Background
Polycarbonate (PC) is a high-quality engineering plastic having excellent overall properties, excellent mechanical properties, high transparency, outstanding weatherability and high-temperature resistance, and good abrasion resistance, dimensional stability and electrical insulation, and thus is widely used in the fields of electronics, electricity, automotive interior and optical media.
In addition, the PC has certain flame retardance, and the flame retardant grade of the general PC resin can reach UL94V2 grade. However, this does not meet the market demands and is therefore of great importance for the modification of PC. Under the conventional conditions, the flame retardant used for flame-retardant modification of the polycarbonate comprises a brominated flame retardant, a phosphorus flame retardant, a silicon flame retardant and a sulfonate flame retardant.
Among them, although the brominated flame retardant has high flame retardant efficiency, the brominated flame retardant contains halogen elements which are easy to be colored and can not meet the environmental protection requirement, so the application of the brominated flame retardant is limited; the addition of the phosphorus flame retardant has certain effect, but can cause the performance of the modified material to be sharply reduced; the sulfonate flame retardant has high efficiency, has little influence on the physical properties of modified materials, and has low influence on the light transmittance of polycarbonate, so the sulfonate flame retardant is favored by researchers; the silicon flame retardant is expensive, but has a good synergistic flame retardant effect, has little influence on the performance of materials, does not change the transparency even when the liquid silicon flame retardant is used, and is a good flame retardant for preparing transparent flame retardant PC. However, in general, it is not sufficient to use a single flame retardant and PTFE, which is an anti-dripping agent, needs to be added, but PTFE affects the transparency of flame-retardant PC, making it difficult for PC to have excellent flame retardancy while ensuring transparency.
In addition, a large amount of bacteria are often bred in the use process of the plastic products, and after a human body contacts the plastic products, the bacteria on the plastic products can be transferred to the human body through contact, so that certain influence is caused on the health of the human body. Therefore, it is a technical problem to be solved urgently at present to provide a transparent polycarbonate material with excellent wear resistance, flame retardancy and antibacterial property.
Disclosure of Invention
Aiming at the defects in the prior art, the first object of the invention is to provide a transparent wear-resistant flame-retardant antibacterial plastic which has good flame-retardant property, light transmittance, antibacterial property and wear resistance.
The second purpose of the invention is to provide a preparation method of the transparent wear-resistant flame-retardant antibacterial plastic, and the prepared plastic has excellent performance and can be widely applied to the manufacture of life-related plastic products.
In order to achieve the first object, the invention provides the following technical scheme:
the transparent wear-resistant flame-retardant antibacterial plastic is characterized by comprising the following components in parts by weight:
by adopting the technical scheme, the PC resin is used as a base material, and the sulfonate flame retardant and the silane flame retardant are added simultaneously, so that when the plastic is ignited, the sulfonate flame retardant can promote the release of carbon dioxide and water, the generation of phenolic substances and the generation of aromatic and aliphatic compounds, further the carbon forming rate of the PC is improved, and the crosslinking of polymers such as PC resin molecules is promoted;
meanwhile, the silane flame retardant can be rapidly transferred to the surface of the material to form a protective layer for oxygen insulation and heat insulation and prevent the lower layer from continuing to burn, and the compound form of the silane flame retardant and the protective layer enables the molecular structure of the PC resin to be better improved, increases the molecular weight of the PC resin and effectively improves the flame retardant property of the plastic; in addition, the molecular weight of the PC resin is increased, so that the dripping of the plastic is reduced, the addition of an anti-dripping agent PTFE is omitted, and the good transparency of the plastic is ensured;
on the basis, an antioxidant, a lubricant, an antibacterial agent and a scratch-resistant agent are added into the PC resin, so that the plastic has more excellent oxidation resistance, antibacterial property and wear resistance.
Further, the PC resin is a isosorbide-type PC resin.
By adopting the technical scheme, the PC resin comprises bisphenol A type PC resin and isosorbide type PC resin, and compared with the traditional bisphenol A type PC resin, the isosorbide type PC resin has a unique alicyclic oxygen structure in a molecular chain, so that the performance is more excellent, and better performances of the material are given, such as high light transmittance, wear resistance and UV aging resistance.
Further, the sulfonate flame retardant is potassium perfluorobutyl sulfonate or potassium diphenylsulfone sulfonate.
By adopting the technical scheme, the potassium perfluorobutyl sulfonate (PFBSK) and the potassium diphenylsulfone sulfonate (KSS) are organic potassium salts, the decomposition rate of PC can be accelerated in the combustion process of the plastic, a carbon layer structure is rapidly formed, oxygen and heat are prevented from being transmitted to the interior of the plastic, and tests prove that the flame retardant can well generate a synergistic effect with a siloxane flame retardant, the flame retardant efficiency when the potassium perfluorobutyl sulfonate (PFBSK) and the flame retardant efficiency when the potassium perfluorobutyl sulfonate (PFBSK) are used are obviously higher than that when one of the two is used alone, and the flame retardant efficiency when the potassium perfluorobutyl sulfonate (PFBSK) is used is higher than that when the potassium diphenylsulfone sulfonate (KSS) is used.
Further, the silane flame retardant is a liquid silicon flame retardant with a structural molecular formula of
Wherein R represents methyl or phenyl, and X represents one of methyl, phenyl, hydroxyl and methoxyl.
By adopting the technical scheme, when the siloxane molecular chain contains methyl, phenyl, hydroxyl and methoxyl, the siloxane molecular chain has the best flame retardant effect on plastics; in addition, because the siloxane flame retardant has good compatibility with PC resin, the addition of the siloxane flame retardant does not reduce other main properties of the material, and can improve the notch impact strength of the material, so that the plastic has excellent mechanical properties.
Further, the antioxidant is compounded by phosphite antioxidant and hindered phenol antioxidant.
By adopting the technical scheme, a synergistic effect exists when the phenolic antioxidant and the phosphite ester are used in combination, active hydrogen atoms exist in molecules of the phenolic antioxidant, the hydrogen atoms are more active than hydrogen atoms (including hydrogen of double bonds on a carbon chain) on a polymer carbon chain, and can be separated out to be combined with macromolecular chain free radicals R & or ROO & to generate hydroperoxide and stable phenolic oxygen free radicals, the hydroperoxide has an automatic catalytic effect on thermal oxidation degradation, the hindered phenol cannot decompose the hydroperoxide per se, the phosphite ester compound does not have the capacity of capturing the peroxide free radicals but can decompose the hydroperoxide, so that the polymer degradation caused by the automatic catalytic reaction is inhibited, and meanwhile, the phosphite ester can also reduce the oxidized phenolic antioxidant. Therefore, when the two are used in combination, the effects complement each other.
Further, the lubricant is one or more of a mixture of stearic acid amide lubricant, hydrocarbon lubricant and fatty acid lubricant.
By adopting the technical scheme, the stearic acid amide lubricant, the hydrocarbon lubricant and the fatty acid lubricant have good compatibility with PC, and mainly play a good role in internal lubrication, and when the flame retardant acts on the PC resin to increase the molecular weight of the PC resin, the flame retardant can better reduce the internal abrasion among resin molecules, thereby ensuring the good structural stability of the PC molecules and having good flame retardant effect. In addition, the stearic acid amide-based lubricant has little influence on the transparency of plastic products and has a great promoting effect on the production of transparent polycarbonate materials, so the lubricant is more preferably the stearic acid amide-based lubricant.
Further, the antibacterial agent is a mixture of an inorganic particle exchanger loaded silver ion antibacterial agent and an organic antibacterial agent.
By adopting the technical scheme, the silver ion antibacterial agent has extremely low hygroscopicity and high heat resistance, is easy to be uniformly dispersed in the PC resin, can generate a synergistic effect with the organic antibacterial agent, and provides good antibacterial performance for plastics.
Further, the scratch-resistant agent is an organic scratch-resistant agent.
By adopting the technical scheme, the organic scratch resistant agent can be better compatible with PC resin compared with the inorganic scratch resistant agent, the migration, precipitation and the like of the organic scratch resistant agent to the surface of plastic are reduced, so that the prepared plastic has good wear resistance, the adverse effect on the impact strength of the plastic caused by adding the inorganic scratch resistant agent into the plastic matrix is avoided, and the compatibility of the scratch resistant agent and the plastic matrix is also improved.
In order to achieve the second object, the invention provides the following technical scheme:
a preparation method of transparent wear-resistant flame-retardant antibacterial plastic comprises the following steps:
(1) weighing the components according to the set weight parts, drying the weighed PC resin at the temperature of 120 ℃ for 4-6h, and drying the other components at the temperature of 50-80 ℃ for 2 h;
(2) putting the dried components into a high-speed mixer, and fully mixing for 5-10min at the temperature of 20-30 ℃;
(3) putting the mixed materials into a double-screw extruder for extrusion granulation, wherein the length-diameter ratio of a screw is 32-40: 1, the temperature of each section of the screw is 240-280 ℃.
By adopting the technical scheme, the components are dried before being fed, so that the performance of the components is ensured, and the interference of moisture on plastics is reduced; and the components are uniformly mixed and then subjected to double-screw extrusion molding, so that the components are uniformly dispersed, the operation is convenient and simple, and the prepared plastic has good flame retardant property, light transmittance, antibacterial property and wear resistance.
Further, in the double-screw extruder, the temperature of the feeding section is 245-265 ℃, the temperature of the melting section is 255-275 ℃, the temperature of the homogenizing section is 260-280 ℃, and the temperature of the head is 260-280 ℃.
By adopting the technical scheme, the temperature in the double screws is gradually increased, so that the components can be fully melted to prevent the components from being placed at high temperature for a long time, thereby reducing the energy output in the extrusion molding process and lowering the production cost.
In conclusion, the invention has the following beneficial effects:
1. according to the invention, the sulfonate flame retardant and the siloxane flame retardant are added into the PC resin at the same time, so that the good transparency of the PC resin is ensured, and the PC resin has good flame retardance; the prepared plastic has good flame retardant property, light transmittance, oxidation resistance, antibacterial property and wear resistance by combining the antioxidant, the lubricant, the antibacterial agent and the scratch-resistant agent;
2. the isosorbide polycarbonate used in the invention has the characteristics of high light transmittance, high surface hardness, good UV aging resistance and the like, and has inherent advantages in preparing transparent wear-resistant flame-retardant polycarbonate;
3. the sulfonate flame retardant is limited to be perfluorobutyl potassium sulfonate or diphenyl sulfone potassium sulfonate, and the silane flame retardant is a liquid silicon flame retardant, so that the flame retardant property of the plastic can be improved, and the mechanical property of the plastic can be improved;
4. the antibacterial agent is defined as a mixture of an inorganic particle exchanger loaded silver ion antibacterial agent and an organic antibacterial agent, and the antibacterial property of the plastic can be effectively improved.
Drawings
FIG. 1 is a process flow diagram for preparing the transparent abrasion-resistant flame-retardant antibacterial plastic of the invention.
Detailed Description
The transparent abrasion-resistant flame-retardant antibacterial plastic and the preparation method thereof are further described in detail in the following with reference to some specific embodiments. The specific examples are intended to illustrate the present invention in further detail, and are not intended to limit the scope of the present invention.
It should be noted that the component materials used in the present invention are commercially available. The embodiment of the invention adopts the following raw materials:
the PC resin is preferably isosorbide type PC resin, and bio-based polycarbonate produced by Mitsubishi corporation is selected.
The sulfonate salt flame retardant is preferably potassium perfluorobutyl sulfonate (PFBSK) or potassium diphenylsulfone sulfonate (KSS); in addition, other sulfonate flame retardants such as sodium 2,4, 5-trichlorobenzenesulfonate (STB) may be used.
The silane flame retardant is preferably a liquid silicon flame retardant with a structural formula of
Wherein R represents methyl or phenyl, and X represents one of methyl, phenyl, hydroxyl and methoxy, such as KR-2710, Polydimethylsiloxane (PDMS), etc.; in addition, other silane flame retardants such as silicone powder may be used.
The antioxidant is a compound of phosphite antioxidant and hindered phenol antioxidant, preferably a compound of antioxidant 618 and antioxidant 1076; antioxidant 618, pentaerythritol dioctadecyl diphosphite, linalool, the content of active substances is 99.99 percent; antioxidant 1076, 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecyl ester, basf, with effective content of 98%.
The lubricant is stearic acid amide, hydrocarbon, fatty acid, preferably stearic acid amide, such as ethylene bis stearic acid amide (EBS), and has small influence on transparency when being added into plastic; EBS, KAOWAX EB, queen flower.
The antibacterial agent is a mixture of an inorganic particle exchanger loaded silver ion antibacterial agent and an organic antibacterial agent, preferably a mixture of a silver ion inorganic glass carrier antibacterial agent and an organic antibacterial agent; wherein, the silver ion inorganic glass carrier antibacterial agent 701S1, Meiling Kangle Million Guard, the content of effective substances is 99 percent; imidazole compounds, BM-2, Shanghai Yue New materials science and technology Limited, active substance content > 95%, decomposition temperature > 350 ℃.
The scratch-resistant agent is preferably an organic scratch-resistant agent, and is further preferably organic polyester graft modified silicone, and compared with an inorganic substance, the organic substance has better compatibility with a plastic matrix; wherein, the polyester graft modified silicone, H-Si6441P, wins special chemical company Limited; SiO 22Milled silica, MIN-U-SIL 5 silica micropowder, U.S. SILICA Quartz Inc. USA, purity 99.5%.
A method for preparing a transparent wear-resistant flame-retardant antibacterial plastic, which is shown in figure 1, and comprises the following steps:
(1) weighing the components according to the set weight parts, drying the weighed PC resin at the temperature of 120 ℃ for 4-6h, and drying the other components at the temperature of 50-80 ℃ for 2 h;
(2) putting the dried components into a high-speed mixer, and fully mixing for 5-10min at the temperature of 20-30 ℃;
(3) and (3) putting the mixed materials into a double-screw extruder for extrusion granulation, wherein the length-diameter ratio of a screw is 32: 1, wherein the temperature of the feeding section is 245-265 ℃, the temperature of the melting section is 255-275 ℃, the temperature of the homogenizing section is 260-280 ℃, and the temperature of the machine head is 260-280 ℃, and finally the transparent wear-resistant flame-retardant antibacterial plastic is obtained.
The plastics obtained were subjected to the following performance tests:
(1) the combustion performance is tested according to UL-94-2006;
(2) the impact strength is tested according to the ASTM D256 standard;
(3) testing the light transmittance according to ASTM D1003-13 standard, wherein the thickness of the test sample is 2.09 mm;
(4) the oxidation resistance is tested according to GB/T19466.6-2009 standard;
(5) and (4) antibacterial property test, wherein the antibacterial property test is carried out by adopting a national film adhesion method, and detection items are escherichia coli and staphylococcus aureus. The antibacterial test piece is 40mm multiplied by 2mm, the test piece is washed clean by distilled water, and the test piece is used for standby after being irradiated by ultraviolet rays. Adding bacterial suspension on each negative and control antibacterial test piece, covering with a sterilized PE film, culturing in a 37 ℃ incubator for 24h, calculating the number of bacterial colonies, repeating the test for 5 times, and averaging the results;
(6) the wear resistance test is carried out, the pencil hardness test is carried out according to the GB/T6739-;
examples 1 to 8 and comparative examples 1 to 4
Examples 1 to 8 and comparative examples 1 to 4 were carried out in the same manner as described above, with the types and amounts of the components and process parameters being adjusted, and the plastics obtained being tested according to the above-described property tests.
Table one composition and weight, unit for examples 1-8 and comparative examples 1-4: kg of
TABLE II test results for examples 1-8 and comparative examples 1-4
In combination with tables one and two, it can be seen from the test results of examples 1 and 8 that the flame retardant property of the plastic produced using the isosorbide type PC resin is V0 grade, while the flame retardant property of the plastic produced using the bisphenol A type PC resin is V1 grade, and at the same time, the light transmittance of the isosorbide type PC resin is also superior to that of the bisphenol A type PC resin, and therefore, the isosorbide type is preferable for the PC resin.
From the test results of example 1, comparative example 1 and comparative example 2, it can be seen that the flame retardant performance of the plastic prepared by adding the sulfonate flame retardant or the silane flame retardant alone can only be maintained at the V2 level, but when the sulfonate flame retardant and the silane flame retardant are used simultaneously, the flame retardant performance of the plastic is improved to the V0 level, the toughness of the plastic is further effectively improved, and the light transmittance is still kept at a higher level.
From the test results of example 1 and example 4 and example 5, it can be seen that when the antioxidant 618 and the antioxidant 1076 are simultaneously used, the improvement of the oxidation resistance of the PC resin is most effective, so that the plastic has excellent oxidation resistance.
From the test results of the example 1, the comparative example 3 and the comparative example 4, when the inorganic carrier silver ion antibacterial agent and the organic antibacterial agent are used simultaneously, the antibacterial property of the plastic can be effectively improved, and under the condition of proper addition amount, the antibacterial rate of the plastic on escherichia coli and staphylococcus aureus reaches 99.9%.
From the test results of example 1 and example 5, it can be seen that the abrasion resistance of the plastic is greatly improved after the addition of the ground silica and the polyester graft modified silicone. However, when silica is added, the impact strength and transparency of the plastic are greatly reduced.
In conclusion, the transparent wear-resistant flame-retardant antibacterial polycarbonate material designed by the invention has good flame retardance, outstanding wear resistance and antibacterial property and good impact property. The material is suitable for plastic products which are in close contact with human skin, such as toys, remote controllers, sanitary wares, computer keyboards and the like.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (5)
1. The transparent wear-resistant flame-retardant antibacterial plastic is characterized by comprising the following components in parts by weight:
100 portions of PC resin
0.03 to 0.12 portion of sulfonate flame retardant
0.2 to 2 portions of silane flame retardant
0.1 to 0.5 portion of antioxidant
0.05 to 0.5 portion of lubricant
0.1 to 1 portion of antibacterial agent
0.75-3 parts of scratch-resistant agent;
the PC resin is isosorbide type PC resin, the antibacterial agent is a mixture of an inorganic particle exchanger loaded silver ion antibacterial agent and an organic antibacterial agent, the sulfonate flame retardant is potassium perfluorobutyl sulfonate, the silane flame retardant is KR-2710, and the scratch-resistant agent is an organic scratch-resistant agent.
2. The transparent wear-resistant flame-retardant antibacterial plastic as claimed in claim 1, wherein the antioxidant is a complex of a phosphite antioxidant and a hindered phenol antioxidant.
3. The transparent abrasion-resistant flame-retardant antibacterial plastic according to claim 1, wherein the lubricant is one or more of a mixture of stearic acid amide type lubricant, hydrocarbon type lubricant and fatty acid type lubricant.
4. The preparation method of the transparent wear-resistant flame-retardant antibacterial plastic according to any one of claims 1 to 3, characterized by comprising the following steps:
(1) weighing the components according to the set weight parts, drying the weighed PC resin at the temperature of 120 ℃ for 4-6h, and drying the other components at the temperature of 50-80 ℃ for 2 h;
(2) putting the dried components into a high-speed mixer, and fully mixing for 5-10min at the temperature of 20-30 ℃;
(3) putting the mixed materials into a double-screw extruder for extrusion granulation, wherein the length-diameter ratio of a screw is 32-40: 1, each section of screw
The temperature is 240 ℃ and 280 ℃.
5. The method as claimed in claim 4, wherein the temperature of the feeding section in the twin-screw extruder is 245-.
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