CN114395237B - Light diffusion flame-retardant PC material capable of being laser-carved and preparation method thereof - Google Patents
Light diffusion flame-retardant PC material capable of being laser-carved and preparation method thereof Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2369/00—Characterised by the use of polycarbonates; Derivatives of polycarbonates
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Abstract
The invention discloses a laser-carving light diffusion PC material which is characterized by comprising the following components in parts by weight: polycarbonate: 83-94 parts; light refraction disruptors: 1-5 parts; self-made flame-retardant master batch: 2-10 parts; toughening agent: 0.2-0.5 part; heat stabilizer: 0.1-0.5 part; and (3) a main antioxidant: 0.1-0.3 part; auxiliary antioxidant: 0.1-0.3 part; ultraviolet absorber: 0.1-0.4 part; light diffusing agent: 0.5-1 part; laser carving auxiliary agent: 0.1-0.5 part; anti-drip agent: 0.05-0.3 parts. The material is processed under a better process condition by adding a compound flame retardant system and proper proportion of other materials, so that the light diffusion PC with excellent flame retardant effect and good laser etching effect is obtained, and is more suitable for being used on lamps.
Description
Technical Field
The invention relates to the field of composite materials, in particular to a laser-carving light diffusion flame-retardant PC material and a preparation method thereof.
Background
With the improvement of life quality requirements, the appearance requirements of people on plastic products related to life are higher and higher, the traditional plastic product surface patterns usually take silk screen printing, spraying and water transfer printing as main manufacturing methods, the obtained patterns are simpler and single, the durability is not strong, in order to obtain appearance effects with better physical properties and higher quality, patterns, numbers, chinese characters and the like are drawn by adopting computer control, the laser carving technology by utilizing a laser marking method is developed through data conduction, the light energy is converted into heat energy by adding a proper laser carving auxiliary agent, the changed and clear patterns are obtained, the time is saved, the energy is saved, and the laser carving technology has been successfully applied to the fields of electronic appliances, livestock ear marks, cosmetic packaging, automobile internal buttons and door handles, instrument boards, computer keyboards, glass lenses, medical devices and the like.
The plastic living products in the market at present are most high-end and diversified in PC application, the Polycarbonate (PC) has higher chemical stability, certain flame retardant property, good heat resistance and transparency, is sensitive to gaps, poor in hydrolysis resistance, poor in organic chemical resistance, poor in scratch resistance, poor in weather resistance, and can yellow after long-term exposure to ultraviolet rays, can be used at a high temperature, has high dimensional stability and good creep resistance, and in order to meet the use environment of PC materials used on lamps, the PC materials generally need to be ensured to have light diffusion effect, flame retardant effect, good light transmittance and aesthetic property, and auxiliaries such as flame retardants can be added into the materials. Under the general condition, the fire retardant influences the transmittance and the haze of the polycarbonate, the transmittance of the light diffusion PC is higher, the infrared light source directly penetrates through the material, the light energy cannot be converted into heat energy in a large amount, and the laser etching effect is difficult to obtain. And because the light is generated, a little light energy is converted into heat energy and is accumulated continuously in the long-term use process, so that the light aging resistance of the material is reduced, and the flame retardant property is poor.
Therefore, a novel laser-engravable light diffusion flame-retardant PC material is needed, and the problems can be solved.
The patent weather-resistant flame-retardant light diffusion PC material for outdoor lamp covers is prepared from, by weight, 81.25-90.17% of PC, 5-15% of toughening agent, 0.8% of light diffusion agent, 1.5-2.5% of flame retardant, 0.4-0.6% of synergistic flame retardant, 0.1-0.5% of hydrolysis inhibitor, 0.1-0.5% of UV inhibitor, 0.03-0.05% of pigment, 0.3% of antioxidant and 0.3% of dispersing agent. The light diffusion PC has good flame retardant effect and weather resistance.
The flame retardant used in the material is an organic silicon flame retardant, the synergistic flame retardant is a sulfonate synergistic flame retardant, and the fluorine-containing carbonate polyurethane elastomer is added as a toughening agent for modification, wherein the hydrolysis-resistant agent and the light stabilizer are added to cause yellowing of the color in the whole formula system, so that the titanium dioxide and the white carbon black with relatively strong covering power are used for adjusting the color, and the whole formula system has better light diffusion and flame retardance effects.
The material has less content of the added flame retardant and cannot be well dispersed, and as the titanium white powder and the white carbon black with strong covering power are added for adjusting the color, the transparency of the product is greatly reduced, and the product affects the laser carving effect, so that the product cannot obtain good appearance patterns.
Disclosure of Invention
The invention aims to provide a novel technical scheme of a light diffusion flame-retardant PC material capable of being laser etched, so that the technical defects that the light diffusion performance is poor and laser etching is difficult in the production and manufacturing process of flame-retardant PC in the prior art are overcome.
According to the first aspect of the invention, a laser-engravable light diffusion PC material is provided, which comprises the following components in parts by mass:
polycarbonate: 83-94 parts;
light refraction disruptors: 1-5 parts;
self-made flame-retardant master batch: 2-10 parts;
toughening agent: 0.2-0.5 part;
heat stabilizer: 0.1-0.5 part;
and (3) a main antioxidant: 0.1-0.3 part;
auxiliary antioxidant: 0.1-0.3 part;
ultraviolet absorber: 0.1-0.4 part;
light diffusing agent: 0.5-1 part;
laser carving auxiliary agent: 0.1-0.5 part;
anti-drip agent: 0.05-0.3 parts.
Preferably, the composition comprises the following components in parts by weight:
polycarbonate: 92 parts;
light refraction disruptors: 2 parts;
self-made flame-retardant master batch: 3.5 parts;
toughening agent: 0.3 parts;
heat stabilizer: 0.3 parts;
and (3) a main antioxidant: 0.2 parts;
auxiliary antioxidant: 0.2 parts;
ultraviolet absorber: 0.15 parts;
light diffusing agent: 0.8 parts;
laser carving auxiliary agent: 0.2 parts;
anti-drip agent: 0.15.
preferably, the self-made flame-retardant master batch comprises the following components in parts by weight:
polycarbonate powder: 100 parts;
potassium perfluorobutyl sulfonate 2025:5 parts;
silsesquioxane flame retardant: 2 parts;
methyl phenyl siloxane: 5 parts;
heat stabilizer: 1 part;
and (3) a main antioxidant: 2 parts;
auxiliary antioxidant: 2 parts.
According to a second aspect of the present invention, there is provided a method for preparing the laser-engravable light-diffusing flame-retardant PC material, which mainly comprises the following steps:
the method comprises the following steps of (1) putting polycarbonate, a light refraction interfering agent, self-made flame-retardant master batch, a toughening agent, an antioxidant, an ultraviolet absorber, a light dispersing agent, an anti-dripping agent and a laser carving auxiliary agent into a high-speed mixer according to parts by weight for mixing;
adding the mixed materials into an extruder for extrusion;
the extruded material strip is cooled to room temperature through a water tank, and the preparation of the light diffusion flame-retardant PC material capable of being subjected to laser engraving is completed through granulation by a granulator.
Preferably, the extruder is a twin-screw extruder with an aspect ratio of 40:1, and the temperature of each temperature zone of the twin-screw extruder is as follows: a section of: 235-245 ℃; two sections: 260-275 ℃; three sections: 260-275 ℃; four sections: 260-275 ℃; five sections: 255-265 ℃; six sections: 255-265 ℃; seven sections: 245-260 ℃; eight sections: 245-260 ℃; nine sections: 245-260 ℃; ten sections: 245-260 ℃; the temperature of the machine head is 245-255 ℃; and the six sections and the nine sections of the extruder are provided with vacuum devolatilizers.
Preferably, the preparation method of the self-made flame-retardant master batch comprises the following steps:
mixing polycarbonate powder and methyl phenyl siloxane, adding silsesquioxane, potassium perfluorobutyl sulfonate, an antioxidant and a heat stabilizer, and mixing again;
mixing uniformly, adding into a double-screw extruder with the length-diameter ratio of 36:1, extruding, cooling the extruded material strips to room temperature through a water tank, and granulating.
Preferably, the temperature of each temperature zone of the twin screw extruder is: a section of: 235-245 ℃; two sections: 240-260 ℃; three sections: 250-265 ℃; four sections: 250-265 ℃; five sections: 250-265 ℃; six sections: 245-255 ℃; seven sections: 245-255 ℃; eight sections: 240-250 ℃; nine sections: 240-250 ℃; the temperature of the machine head is 240-250 ℃.
In the laser engraving process, the carbonized material absorbs heat when engraving black fonts, the material of the engraved part is foamed when engraving white fonts, and under the general conditions, brominated flame retardants, carbon black, titanium pigment and white carbon black have larger influence on the laser engraving effect, and transparent products can not convert light energy into heat energy because of light transmission.
The flame-retardant system used in the patent has smaller influence on the laser carving effect on the premise of ensuring the flame-retardant effect, and is more suitable for being used on lamps;
the material adopts a compound flame retardant system, so that the flame retardant efficiency is improved, meanwhile, the smoke quantity and the toxic gas release quantity can be greatly reduced when the material is heated and combusted, the environmental pollution is reduced, the corrosiveness of the material to an injection mold is low, the processing cost is reduced, and the choking condition caused by human smoke can be reduced when fire disaster occurs due to the low VOC content of the material, so that the safety performance can be greatly improved;
the patent uses the flame-retardant system compounded by the potassium perfluorobutyl sulfonate, the silsesquioxane and the transparent methyl phenyl siloxane with less addition, and the flame-retardant system is a reactive flame retardant, so that the addition is less, and the influence of the flame retardant on the laser carving effect is reduced. In addition, because the light transmittance of the transparent product is larger, the light energy cannot be gathered, so that the transparent light diffusion PC cannot be well converted into heat energy, and the transparent light diffusion PC cannot be well engraved with patterns even though the laser engraving auxiliary agent is added, so that a small amount of transparent light refraction interference agent is introduced to change the refractive index of the PC, so that the haze of the surface of the product is changed, laser engraving is facilitated, and the light source of the material in the production of the PC lampshade is softer and brighter. Meanwhile, laser etching auxiliary agent powder which is more suitable for transparent materials is added, so that a light diffusion flame-retardant PC material which is more suitable for laser etching is obtained;
the material uses potassium perfluorobutyl sulfonate 2025 as a main flame retardant, and silsesquioxane QB-C02 and methyl phenyl siloxane reactive high-performance liquid additives are used as auxiliary flame retardants in a synergistic and compounding way, so that the reduction of physical properties such as elongation at break, ductility, surface tension, heat resistance, impact, rigidity and the like of the material caused by adding other flame retardants and auxiliary products is greatly improved, the Flame Retardance (FR) of the polycarbonate is improved, the high definition of minimum haze is reserved, and the transparency of the polycarbonate is hardly affected;
other features of the present invention and its advantages will become apparent from the following detailed description of exemplary embodiments of the invention.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail. It should be noted that: the relative arrangement of the components and steps, numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless it is specifically stated otherwise.
The following description of at least one exemplary embodiment is merely exemplary in nature and is in no way intended to limit the invention, its application, or uses.
Techniques, methods, and apparatus known to one of ordinary skill in the relevant art may not be discussed in detail, but are intended to be part of the specification where appropriate.
In all examples shown and discussed herein, any specific values should be construed as merely illustrative, and not a limitation. Thus, other examples of exemplary embodiments may have different values.
Example 1
The laser-engravable light diffusion PC material comprises the following components in parts by mass:
polycarbonate: 83-94 parts;
light refraction disruptors: 1-5 parts;
self-made flame-retardant master batch: 2-10 parts;
toughening agent: 0.2-0.5 part;
heat stabilizer: 0.1-0.5 part;
and (3) a main antioxidant: 0.1-0.3 part;
auxiliary antioxidant: 0.1-0.3 part;
ultraviolet absorber: 0.1-0.4 part;
light diffusing agent: 0.5-1 part;
laser carving auxiliary agent: 0.1-0.5 part;
anti-drip agent: 0.05-0.3.
The self-made flame-retardant master batch in the embodiment comprises the following components in parts by mass:
polycarbonate powder: 100 parts;
potassium perfluorobutyl sulfonate 2025:5 parts;
silsesquioxane QB-C02:2 parts;
methyl phenyl siloxane: 5 parts;
heat stabilizer: 1 part;
and (3) a main antioxidant: 2 parts;
auxiliary antioxidant: 2 parts.
Wherein the polycarbonate is a high viscosity polycarbonate PC110; the light refraction disrupter is ABS920; the toughening agent is maleic anhydride modified polyethylene wax 1105A; the heat stabilizer is C-10RW; the main antioxidant of the beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) octadecyl propionate is 1076; the phosphite auxiliary antioxidant is 168; the high molecular weight hydroxyphenyl benzotriazole ultraviolet absorber is UV-234; the Japanese ponding light diffusion agent is EXM-5; the laser carving auxiliary agent is merck 8825; the anti-drip agent is Polytetrafluoroethylene (PTFE).
Under the condition that a small molecular lubricant with degradation promoting effect is not additionally added, the PC is modified by using a wax transparent dispersion toughening agent with a macromolecular chain, the addition amount is small, the product permeability and haze are not influenced, and the good self-lubricating effect can enable flame-retardant master batches and other auxiliary agents to obtain better dispersion effect in a screw rod while toughening, so that a flame-retardant polycarbonate product with good environmental stress cracking resistance can be obtained, particularly for products of screw inserts, the phenomenon of stress concentration is weakened, and cracking caused by the excessive concentration of stress around screws is avoided;
the ultraviolet absorber has the advantages that the ultraviolet absorber is low in volatility, high in light absorption, good in compatibility with base materials, low in volatility and difficult to hydrolyze, and can be used for preparing powdery heat stabilizer C-10RW, the ultraviolet absorber is good in light aging resistance, and yellowing resistance is achieved under outdoor conditions. The heat stabilizer can effectively resist polymer degradation, yellowing and fading caused by shearing and hot pressing force in the processing process, and can be used as a synergistic heat stabilizer together with an antioxidant, so that the performance of the end group is more stable, the depolymerization at high temperature is not easy, and the service life of the polymer is prolonged under the condition of thermal aging. As the two proper photo-thermal aging system products are added, the surface of the product does not yellow or precipitate after long-term use, and the long-term use of the product is not affected.
The flame-retardant system in the patent is a flame-retardant composite system of potassium perfluorobutyl sulfonate 2025, silsesquioxane QB-C02 and methyl phenyl siloxane. The product produced by the flame-retardant system has no influence on transparency, and the material has higher heat resistance, and besides the addition of the reactive potassium perfluorobutyl sulfonate, the better flame-retardant light diffusion PC capable of laser carving is obtained by utilizing the synergistic effect of silsesquioxane, methyl phenyl siloxane and a main flame-retardant system.
The flame retardant is added in a smaller amount, so that the polycarbonate and the flame retardant are mixed uniformly, the obtained flame retardant master batch is better in dispersing effect, and the flame retardant is prepared into particles in advance and added, so that the flame retardant is easier to disperse uniformly.
Because the flame retardant has an influence on the laser etching powder, the energy can be instantly dispersed by adding the flame retardant, the energy can be accumulated by the laser etching auxiliary agent, the influence of the brominated flame retardant on the laser etching is relatively large, and the influence of the reactive flame retardant which does not contain bromine and chlorine and is used in the patent on the laser etching effect is relatively small, and the smaller the adding amount is, the smaller the influence is. After the brominated flame-retardant PC is added with the light diffusion agent, the long-term light diffusion effect cannot be achieved, the transmittance of the light source is reduced rapidly, and after the brominated flame-retardant PC is added with the laser etching powder, etching is not easy, and the fonts are not clear. Therefore, the traditional method for producing transparent polycarbonate by using brominated flame retardant modified Polycarbonate (PC) is changed, and the brominated flame retardant and the chlorine-free flame retardant are used, so that the light source is better dispersed, and the product has better laser engraving effect.
The preparation method of the laser-etching light diffusion flame-retardant PC material mainly comprises the following steps:
the method comprises the steps of (1) putting polycarbonate, a light refraction interfering agent ABS920, self-made flame-retardant master batch, a toughening agent, an antioxidant, an ultraviolet absorber, a light dispersing agent, an anti-dripping agent and a laser carving auxiliary agent into a high-speed mixer according to parts by weight, uniformly mixing for 3 minutes, and adding the uniformly mixed materials into an extruder for extrusion; the extruded material strip is cooled to room temperature through a water tank, and the preparation of the light diffusion flame-retardant PC material capable of being subjected to laser engraving is completed through granulation by a granulator.
The extruder is a double-screw extruder with the length-diameter ratio of 40:1, and the temperature of each temperature zone of the double-screw extruder is as follows: a section of: 235-245 ℃; two sections: 260-275 ℃; three sections: 260-275 ℃; four sections: 260-275 ℃; five sections: 255-265 ℃; six sections: 255-265 ℃; seven sections: 245-260 ℃; eight sections: 245-260 ℃; nine sections: 245-260 ℃; ten sections: 245-260 ℃; the temperature of the machine head is 245-255 ℃;
the polycarbonate is thermoplastic, is sensitive to shearing heat, and in order to reduce the generation of the shearing heat, the processing temperature of a melting section from a feed opening to four areas is set to be high-temperature processing, so that the polycarbonate material can be rapidly melted in a double-screw extruder, the shearing heat of the double-screw extruder to the material is reduced, the torque of the screw is reduced, the loss of equipment is further reduced, meanwhile, the polycarbonate material can be well dispersed in a shearing section, the processing temperature of the shearing section and a dispersing section is reduced, and the degradation of the polycarbonate material is reduced.
The six sections and the nine sections of the extruder are provided with vacuum devolatilizers to realize double-vacuum control, thereby improving and controlling the odor of the modified product and the volatilization of harmful substances thereof.
Before production, the polycarbonate needs to be dried at 120 ℃ for 4-6 hours, after the materials are mixed, the polycarbonate needs to be sealed, and the polycarbonate is used as soon as possible, so that the polycarbonate is prevented from absorbing moisture again, and after the material is granulated, the material is cooled in water at 40 ℃ and immediately leaves water, so that the hydrolysis phenomenon in the production process is prevented, and the performance of the material is prevented from being influenced.
The preparation method of the self-made flame-retardant master batch in the embodiment is as follows:
uniformly mixing polycarbonate powder and methyl phenyl siloxane (liquid) for 2 minutes, uniformly adding a flame retardant potassium perfluorobutyl sulfonate, a silsesquioxane flame retardant, an antioxidant and a heat stabilizer into the mixed polycarbonate according to parts by weight, and uniformly mixing for 2 minutes again; mixing uniformly, adding into a double-screw extruder with the length-diameter ratio of 36:1, extruding, cooling the extruded material strips to room temperature through a water tank, and granulating.
Wherein the temperature of each temperature zone of the twin-screw extruder is as follows: a section of: 235-245 ℃; two sections: 240-260 ℃; three sections: 250-265 ℃; four sections: 250-265 ℃; five sections: 250-265 ℃; six sections: 245-255 ℃; seven sections: 245-255 ℃; eight sections: 240-250 ℃; nine sections: 240-250 ℃; the temperature of the machine head is 240-250 ℃.
In order to reduce the problem that the self-made flame-retardant master batch is subjected to thermal degradation due to shearing heat by a double-screw extruder, so that the material performance is affected, a 36:1 double-screw extruder with a relatively short length-diameter ratio is used, and meanwhile, methyl phenyl siloxane is easy to volatilize at high temperature, so that low-temperature processing with gradual heating is used in a first area and a second area of a feed opening, volatilization of a liquid flame-retardant synergist is reduced, rapid heating is carried out in a third area to a fifth area, a polycarbonate material is rapidly melted, and dispersion of the flame retardant in the double-screw extruder is accelerated. After dispersing various auxiliary materials, extruding at a machine head at a low temperature, reducing thermal degradation of the materials, and preserving excellent physical and chemical properties for reprocessing.
Example 2
The laser-etching light diffusion PC material in the embodiment comprises the following components in parts by mass:
polycarbonate: 83 parts;
light refraction disruptors: 5 parts;
self-made flame-retardant master batch: 10 parts;
toughening agent: 0.2 parts;
heat stabilizer: 0.1 part;
and (3) a main antioxidant: 0.1 part;
auxiliary antioxidant: 0.3 parts;
ultraviolet absorber: 0.4 parts;
light diffusing agent: 0.5 parts;
laser carving auxiliary agent: 0.1 part;
anti-drip agent: 0.3 parts.
Wherein the polycarbonate is a high viscosity polycarbonate PC110; the light refraction disrupter is ABS920; the toughening agent is maleic anhydride modified polyethylene wax 1105A; the heat stabilizer is C-10RW; the main antioxidant of the beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) octadecyl propionate is 1076; the phosphite auxiliary antioxidant is 168; the high molecular weight hydroxyphenyl benzotriazole ultraviolet absorber is UV-234; the Japanese ponding light is diffused into EXM-5; the laser carving auxiliary agent is merck 8825; the anti-drip agent is Polytetrafluoroethylene (PTFE).
The flame-retardant master batch in the embodiment comprises the following components in parts by mass:
polycarbonate powder: 100 parts;
potassium perfluorobutyl sulfonate 2025:5 parts;
silsesquioxane QB-C02:2 parts;
methyl phenyl siloxane: 5 parts;
heat stabilizer: 1 part;
and (3) a main antioxidant: 2 parts;
auxiliary antioxidant: 2 parts.
Wherein the flame-retardant system is a flame-retardant composite system of potassium perfluorobutyl sulfonate 2025, silsesquioxane QB-C02 and methyl phenyl siloxane. An experimental part was prepared according to the preparation method in example 1.
Example 3
The laser-engravable light diffusion PC material comprises the following components in parts by mass:
polycarbonate: 94 parts;
light refraction disruptors: 1 part;
self-made flame-retardant master batch: 2 parts;
toughening agent: 0.5 parts;
heat stabilizer: 0.5 parts;
and (3) a main antioxidant: 0.3 parts;
auxiliary antioxidant: 0.1 part;
ultraviolet absorber: 0.1 part;
light diffusing agent: 1 part;
laser carving auxiliary agent: 0.5 parts;
anti-drip agent: 0.05 part.
Wherein the polycarbonate is a high viscosity polycarbonate PC110; the light refraction disrupter is ABS920; the toughening agent is maleic anhydride modified polyethylene wax 1105A; the heat stabilizer is C-10RW; the main antioxidant of the beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) octadecyl propionate is 1076; the phosphite auxiliary antioxidant is 168; the high molecular weight hydroxyphenyl benzotriazole ultraviolet absorber is UV-234; the Japanese ponding light is diffused into EXM-5; the merck laser carving auxiliary agent is 8825; the anti-drip agent is Polytetrafluoroethylene (PTFE).
The self-made flame-retardant master batch in the embodiment comprises the following components in parts by mass:
polycarbonate powder: 100 parts;
potassium perfluorobutyl sulfonate 2025:5 parts;
silsesquioxane QB-C02:2 parts;
methyl phenyl siloxane: 5 parts;
heat stabilizer: 1 part;
and (3) a main antioxidant: 2 parts;
auxiliary antioxidant: 2 parts.
Wherein the flame-retardant system is a flame-retardant composite system of potassium perfluorobutyl sulfonate 2025, silsesquioxane QB-C02 and methyl phenyl siloxane. An experimental part was prepared according to the preparation method in example 1.
Example 4
The laser-engravable light diffusion PC material comprises the following components in parts by mass:
polycarbonate: 92 parts;
light refraction disruptors: 2 parts;
self-made flame-retardant master batch: 3.5 parts;
toughening agent: 0.3 parts;
heat stabilizer: 0.3 parts;
and (3) a main antioxidant: 0.2 parts;
auxiliary antioxidant: 0.2 parts;
ultraviolet absorber: 0.15 parts;
light diffusing agent: 0.8 parts;
laser carving auxiliary agent: 0.2 parts;
anti-drip agent: 0.15 parts.
Wherein the polycarbonate is a high viscosity polycarbonate PC110; the light refraction disrupter is ABS920; the toughening agent is maleic anhydride modified polyethylene wax 1105A; the heat stabilizer is C-10RW; the main antioxidant of the beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) octadecyl propionate is 1076; the phosphite auxiliary antioxidant is 168; the high molecular weight hydroxyphenyl benzotriazole ultraviolet absorber is UV-234; the Japanese ponding light is diffused into EXM-5; the merck laser carving auxiliary agent is 8825; the anti-drip agent is Polytetrafluoroethylene (PTFE).
The self-made flame-retardant master batch in the embodiment comprises the following components in parts by mass:
polycarbonate powder: 100 parts;
potassium perfluorobutyl sulfonate 2025:5 parts;
silsesquioxane QB-C02:2 parts;
methyl phenyl siloxane: 5 parts;
heat stabilizer: 1 part;
and (3) a main antioxidant: 2 parts;
auxiliary antioxidant: 2 parts.
Wherein the flame-retardant system is a flame-retardant composite system of potassium perfluorobutyl sulfonate 2025, silsesquioxane QB-C02 and methyl phenyl siloxane. Homemade flame retardant master batches were prepared according to the preparation method in example 1.
Comparative example 1
The laser-engravable light diffusion PC material comprises the following components in parts by mass:
polycarbonate: 92 parts;
light refraction disruptors: 2 parts;
self-made flame-retardant master batch: 3.5 parts;
toughening agent: 0.3 parts;
heat stabilizer: 0.3 parts;
and (3) a main antioxidant: 0.2 parts;
auxiliary antioxidant: 0.2 parts;
ultraviolet absorber: 0.15 parts;
light diffusing agent: 0.8 parts;
laser carving auxiliary agent: 0.2 parts;
anti-drip agent: 0.15 parts.
Titanium white powder: 1 part of
Wherein the polycarbonate is a high viscosity polycarbonate PC110; the light refraction disrupter is ABS920; the toughening agent is maleic anhydride modified polyethylene wax 1105A; the heat stabilizer is C-10RW; the main antioxidant of the beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) octadecyl propionate is 1076; the phosphite auxiliary antioxidant is 168; the high molecular weight hydroxyphenyl benzotriazole ultraviolet absorber is UV-234; the Japanese ponding light is diffused into EXM-5; the merck laser carving auxiliary agent is 8825; the anti-dripping agent is Polytetrafluoroethylene (PTFE); the titanium white powder is DuPont R105.
The self-made flame-retardant master batch in the embodiment comprises the following components in parts by mass:
polycarbonate powder: 100 parts;
potassium perfluorobutyl sulfonate 2025:5 parts;
silsesquioxane QB-C02:2 parts;
methyl phenyl siloxane: 5 parts;
heat stabilizer: 1 part;
and (3) a main antioxidant: 2 parts;
auxiliary antioxidant: 2 parts.
Wherein the flame-retardant system is a flame-retardant composite system of potassium perfluorobutyl sulfonate 2025, silsesquioxane QB-C02 and methyl phenyl siloxane. Homemade flame retardant master batches were prepared according to the preparation method in example 1.
Comparative example 2
The laser-engravable light diffusion PC material comprises the following components in parts by mass:
polycarbonate: 94 parts;
self-made flame-retardant master batch: 3.5 parts;
toughening agent: 0.3 parts;
heat stabilizer: 0.3 parts;
and (3) a main antioxidant: 0.2 parts;
auxiliary antioxidant: 0.2 parts;
ultraviolet absorber: 0.15 parts;
light diffusing agent: 0.8 parts;
laser carving auxiliary agent: 0.2 parts;
anti-drip agent: 0.15 parts.
Wherein the polycarbonate is a high viscosity polycarbonate PC110; the toughening agent is maleic anhydride modified polyethylene wax 1105A; the heat stabilizer is C-10RW; the main antioxidant of the beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) octadecyl propionate is 1076; the phosphite auxiliary antioxidant is 168; the high molecular weight hydroxyphenyl benzotriazole ultraviolet absorber is UV-234; the Japanese ponding light diffusion agent is EXM-5; the laser carving auxiliary agent is merck 8825; the anti-drip agent is Polytetrafluoroethylene (PTFE).
The whole formula is a material prepared under the condition of not adding a light refraction interference agent, namely not adding ABS 920.
The self-made flame-retardant master batch in the embodiment comprises the following components in parts by mass:
polycarbonate powder: 100 parts;
potassium perfluorobutyl sulfonate 2025:5 parts;
silsesquioxane QB-C02:2 parts;
methyl phenyl siloxane: 5 parts;
heat stabilizer: 1 part;
and (3) a main antioxidant: 2 parts;
auxiliary antioxidant: 2 parts.
Wherein the flame-retardant system is a flame-retardant composite system of potassium perfluorobutyl sulfonate 2025, silsesquioxane QB-C02 and methyl phenyl siloxane. An experimental part was prepared according to the preparation method in example 1.
Comparative example 3
The laser-engravable light diffusion PC material comprises the following components in parts by mass:
polycarbonate: 87 parts;
light refraction disruptors: 2 parts of
Self-made flame-retardant master batch: 10 parts;
toughening agent: 0.3 parts;
heat stabilizer: 0.3 parts;
and (3) a main antioxidant: 0.2 parts;
auxiliary antioxidant: 0.2 parts;
ultraviolet absorber: 0.15 parts;
light diffusing agent: 0.8 parts;
laser carving auxiliary agent: 0.2 parts;
anti-drip agent: 0.15 parts.
Wherein the polycarbonate is a high viscosity polycarbonate PC110; the light refraction disrupter is ABS920; the toughening agent is maleic anhydride modified polyethylene wax 1105A; the heat stabilizer is C-10RW; the main antioxidant of the beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) octadecyl propionate is 1076; the phosphite auxiliary antioxidant is 168; the high molecular weight hydroxyphenyl benzotriazole ultraviolet absorber is UV-234; the Japanese ponding light is diffused into EXM-5; the merck laser carving auxiliary agent is 8825; the anti-drip agent is Polytetrafluoroethylene (PTFE).
The self-made flame-retardant master batch in the embodiment comprises the following components in parts by mass:
polycarbonate powder: 100 parts;
bisphenol a bis (diphenyl phosphate) (BDP): 35 parts;
potassium perfluorobutyl sulfonate 2025:5 parts;
heat stabilizer: 1 part;
and (3) a main antioxidant: 2 parts;
auxiliary antioxidant: 2 parts.
The preparation method of the self-made flame-retardant master batch comprises the following steps:
mixing polycarbonate powder, potassium perfluorobutyl sulfonate, an antioxidant and a heat stabilizer; bisphenol a bis (diphenyl phosphate) (BDP) was added in the five zones by a side feed liquid metering device (hydraulic).
Extruding the uniformly mixed materials in a double-screw extruder with the length-diameter ratio of 36:1, cooling the extruded material strips to room temperature through a water tank, and granulating.
Preferably, the temperature of each temperature zone of the twin screw extruder is: a section of: a section of: 235-245 ℃; two sections: 260-275 ℃; three sections: 260-275 ℃; four sections: 260-275 ℃; five sections: 240-255 ℃; six sections: 255-265 ℃; seven sections: 255-265 ℃; eight sections: 240-250 ℃; nine sections: 240-250 ℃; the temperature of the machine head is 240-250 ℃.
The processing temperature is that one to four areas are adopted to rapidly melt the polycarbonate powder at high temperature, the materials are completely melted before the liquid is added, the dispersion of the auxiliary agent and the flame retardant is facilitated in the shearing dispersion section, the temperature is reduced at the inlet of the five-section liquid feed, the degradation degree is prevented from being increased by adding BDP at high temperature, and the loss of BDP is increased in the vaporization process.
Comparative example 4
The laser-engravable light diffusion PC material comprises the following components in parts by mass:
polycarbonate: 87 parts;
light refraction disruptors: 2 parts of
Self-made flame-retardant master batch: 10 parts;
toughening agent: 0.3 parts;
heat stabilizer: 0.3 parts;
and (3) a main antioxidant: 0.2 parts;
auxiliary antioxidant: 0.2 parts;
ultraviolet absorber: 0.15 parts;
light diffusing agent: 0.8 parts;
laser carving auxiliary agent: 0.2 parts;
anti-drip agent: 0.15 parts.
Wherein the polycarbonate is a high viscosity polycarbonate PC110; the light refraction disrupter is ABS920; the toughening agent is maleic anhydride modified polyethylene wax 1105A; the heat stabilizer is C-10RW; the main antioxidant of the beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) octadecyl propionate is 1076; the phosphite auxiliary antioxidant is 168; the high molecular weight hydroxyphenyl benzotriazole ultraviolet absorber is UV-234; the Japanese ponding light is diffused into EXM-5; the merck laser carving auxiliary agent is 8825; the anti-drip agent is Polytetrafluoroethylene (PTFE).
The flame-retardant master batch in the embodiment comprises the following components in parts by mass:
polycarbonate powder: 100 parts;
bromotriazine (245): 70 parts;
heat stabilizer: 1 part;
and (3) a main antioxidant: 2 parts;
auxiliary antioxidant: 2 parts.
Wherein the flame retardant system is a bromotriazine single brominated system. Preferably, the preparation method of the flame retardant masterbatch comprises the following steps:
mixing polycarbonate powder, bromotriazine, an antioxidant and a heat stabilizer; mixing uniformly, adding into a double-screw extruder with the length-diameter ratio of 36:1, extruding, cooling the extruded material strips to room temperature through a water tank, and granulating.
Preferably, the temperature of each temperature zone of the twin screw extruder is: a section of: a section of: 235-245 ℃; two sections: 260-275 ℃; three sections: 260-275 ℃; four sections: 260-275 ℃; five sections: 240-255 ℃; six sections: 245-255 ℃; seven sections: 245-255 ℃; eight sections: 240-250 ℃; nine sections: 240-250 ℃; the temperature of the machine head is 240-250 ℃.
The processing temperature is that the first half section adopts high temperature melting materials to accelerate the dispersion of the shearing section, and the fifth section is produced normally according to the conventional process to reduce the thermal degradation of the materials.
Comparative example 5
The laser-engravable light diffusion PC material comprises the following components in parts by mass:
polycarbonate: 94 parts;
light refraction disruptors: 2 parts of
Self-made flame-retardant master batch: 3.5 parts;
toughening agent: 0.3 parts;
heat stabilizer: 0.3 parts;
and (3) a main antioxidant: 0.2 parts;
auxiliary antioxidant: 0.2 parts;
ultraviolet absorber: 0.15 parts;
light diffusing agent: 0.8 parts;
laser carving auxiliary agent: 0.2 parts;
anti-drip agent: 0.15 parts.
Wherein the polycarbonate is a high viscosity polycarbonate PC110; the light refraction disrupter is ABS920; the toughening agent is maleic anhydride modified polyethylene wax 1105A; the heat stabilizer is C-10RW; the main antioxidant of the beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) octadecyl propionate is 1076; the phosphite auxiliary antioxidant is 168; the high molecular weight hydroxyphenyl benzotriazole ultraviolet absorber is UV-234; the Japanese ponding light is diffused into EXM-5; changing the laser engraving auxiliary agent into a domestic model; the anti-drip agent is Polytetrafluoroethylene (PTFE).
The self-made flame-retardant master batch in the embodiment comprises the following components in parts by mass:
polycarbonate powder: 100 parts;
potassium perfluorobutyl sulfonate 2025:5 parts;
silsesquioxane QB-C02:2 parts;
methyl phenyl siloxane: 5 parts;
heat stabilizer: 1 part;
and (3) a main antioxidant: 2 parts;
auxiliary antioxidant: 2 parts.
Wherein the flame-retardant system is a flame-retardant composite system of potassium perfluorobutyl sulfonate 2025, silsesquioxane QB-C02 and methyl phenyl siloxane. An experimental part was prepared according to the preparation method in example 1.
Comparative example 6
The laser-engravable light diffusion PC material comprises the following components in parts by mass:
polycarbonate: 91 parts;
light refraction disruptors: 2 parts of
Self-made flame-retardant master batch: 3.5 parts;
toughening agent: 3 parts;
heat stabilizer: 0.3 parts;
and (3) a main antioxidant: 0.2 parts;
auxiliary antioxidant: 0.2 parts;
ultraviolet absorber: 0.15 parts;
light diffusing agent: 0.8 parts;
laser carving auxiliary agent: 0.2 parts;
anti-drip agent: 0.15 parts.
Wherein the polycarbonate is a high viscosity polycarbonate PC110; the light refraction disrupter is ABS920; the toughening agent is polymethyl methacrylate-butadiene-styrene terpolymer (MBS); the heat stabilizer is C-10RW; the main antioxidant of the beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) octadecyl propionate is 1076; the phosphite auxiliary antioxidant is 168; the high molecular weight hydroxyphenyl benzotriazole ultraviolet absorber is UV-234; the Japanese ponding light is diffused into EXM-5; the merck laser carving auxiliary agent is 8825; the anti-drip agent is Polytetrafluoroethylene (PTFE).
The self-made flame-retardant master batch in the embodiment comprises the following components in parts by mass:
polycarbonate powder: 100 parts;
potassium perfluorobutyl sulfonate 2025:5 parts;
silsesquioxane QB-C02:2 parts;
methyl phenyl siloxane: 5 parts;
heat stabilizer: 1 part;
and (3) a main antioxidant: 2 parts;
auxiliary antioxidant: 2 parts.
Wherein the flame-retardant system is a flame-retardant composite system of potassium perfluorobutyl sulfonate 2025, silsesquioxane QB-C02 and methyl phenyl siloxane. An experimental part was prepared according to the preparation method in example 1.
The results of comparing the experimental parts of examples 2 to 4 with those of comparative examples 1 to 6 in terms of melt flow rate, elongation at break, notched Izod impact strength, glow wire, 1.4mm haze, 1.4mm transmittance, xenon lamp radiation exposure, flame retarding effect, appearance color, laser engraving effect and the like are shown in Table 1
Table 1 comparison of the parameters of the experimental materials in examples 2 to 4 and comparative examples 1 to 6
Correlation test methods and criteria:
1. melt flow rate: GB/T1033;
2. elongation at break: ISO 527;
3. notched impact strength of cantilever beam GB/T1843
4. Glow wire: IEC 60695-2-12;
5. haze, ASTM D-1003-2007;
6. full light transmittance: DIN 5036-1;
7. flame retardant UL94-2006;
8. xenon lamp artificial weathering test, second part of the light source test method in plastics laboratory: xenon arc lamps, GB/T16422.2-1999;
9. laser etching test: aiming at 1060nm near infrared laser, the mark is clear, sharp, fast and high in contrast.
As can be seen from the data in the table, in example 2 and example 3, the former is influenced by the more of the added self-made flame retardant master batch and the ABS light interference agent, while the flame retardant property of the material is better, the surface of the product is white, the light source is yellow, the laser etching effect is influenced by the flame retardant, the laser etching agent is less, the whole laser etching effect is not very good, and the light diffusion effect is poorer than that of example 3 in example 2. The auxiliary materials in the embodiment 4 are suitable in proportion, and the product has moderate surface permeability and haze, soft light source, higher physical property, better laser engraving effect, better impact strength, good weather resistance, higher glowing filament use temperature and better light diffusion effect. In comparative example 1, 1 part of titanium dioxide is added on the basis of example 4, the melt flow rate, the elongation at break and the impact strength are all reduced, the transmittance is reduced, the haze is larger, the light source is whiter, and the light diffusion effect of the material is weaker than that of example 4 and becomes worse due to the fact that the titanium dioxide is introduced, and the laser engraving effect is poor. In the comparative example 2, ABS with light interference is not added, so that even if light stabilizer is added, the surface of the material is light-transmitting beads, and the light source is not soft enough and the brightness is enough in the daily use process, but the material is glaring when directly looking at the light source. And because the transparency is too high, the light source transmittance is too high, the light energy can not be converted into heat energy, the laser carving effect is poor, and the light diffusion effect is poor. In comparative example 3, since the liquid flame retardant is added, unlike the reactive flame retardants of sulfonate, potassium perfluorobutyl sulfonate and silsesquioxane, the addition amount is relatively large, and has a relatively large influence on the heat distortion temperature and the use temperature of a glow wire of the material, and the larger the addition amount, the lower the impact strength, the worse the heat resistance, the good light diffusion effect and the general laser engraving effect. In comparative example 4, the impact strength of the whole material is greatly affected because of the use of the brominated flame retardant system, and the flame retardant efficiency of the flame retardant is lower than that of the flame retardants such as sulfonate, potassium perfluorobutyl sulfonate, silsesquioxane and the like, so that the flame retardant effect is poor, the laser etching effect is poor because of the relatively large influence of the brominated flame retardant on the laser etching effect, and the use temperature of the glowing filament is low. The light source is soft, the color is easy to change during high-temperature processing, and the light diffusion effect is poor. In comparative column 5, the laser engraving powder is transparent pale yellow powder, the product has moderate transmittance and haze, the surface is yellow, the light source is warm light, the laser engraving effect is poor, but the light diffusion effect is good. In comparative example 6, the toughening agent of polymethyl methacrylate-butadiene-styrene (MBS) is used, so that the toughening agent affects the transparency and haze of the product, the toughening agent is not easy to disperse in a formula system due to the fact that the content of glue is too high, the dispersing requirement on a screw in the processing process is relatively high, the product is low in transparency, high in haze and weak in dispersing effect, but the MBS is easy to burn and easy to gather energy, so that the laser engraving effect is good, and the light dispersing effect is poor.
While certain specific embodiments of the invention have been described in detail by way of example, it will be appreciated by those skilled in the art that the above examples are for illustration only and are not intended to limit the scope of the invention. It will be appreciated by those skilled in the art that modifications may be made to the above embodiments without departing from the scope and spirit of the invention. The scope of the invention is defined by the appended claims.
Claims (2)
1. The laser-engravable light diffusion PC material is characterized by comprising the following components in parts by weight:
polycarbonate: 92 parts;
light refraction disruptors: 2 parts;
self-made flame-retardant master batch: 3.5 parts;
toughening agent: 0.3 parts;
heat stabilizer: 0.3 parts;
and (3) a main antioxidant: 0.2 parts;
auxiliary antioxidant: 0.2 parts;
ultraviolet absorber: 0.15 parts;
light diffusing agent: 0.8 parts;
laser carving auxiliary agent: 0.2 parts;
anti-drip agent: 0.15;
the self-made flame-retardant master batch comprises the following components in parts by weight:
polycarbonate powder: 100 parts;
potassium perfluorobutyl sulfonate 2025:5 parts;
silsesquioxane flame retardant: 2 parts;
methyl phenyl siloxane: 5 parts;
heat stabilizer: 1 part;
and (3) a main antioxidant: 2 parts;
auxiliary antioxidant: 2 parts.
2. A method for preparing the laser-etched light-diffusing PC material according to claim 1, which is characterized by mainly comprising the following steps:
the method comprises the following steps of (1) putting polycarbonate, a light refraction interfering agent, self-made flame-retardant master batch, a toughening agent, an antioxidant, an ultraviolet absorber, a light dispersing agent, an anti-dripping agent and a laser carving auxiliary agent into a high-speed mixer according to parts by weight for mixing;
adding the mixed materials into an extruder for extrusion;
the extruded material strip is cooled to room temperature through a water tank, and the preparation of the light diffusion flame-retardant PC material capable of being subjected to laser engraving is completed through granulation by a granulator; the extruder is a double-screw extruder with the length-diameter ratio of 40:1, and the temperature of each temperature zone of the double-screw extruder is as follows: a section of: 235-245 ℃; two sections: 260-275 ℃; three sections: 260-275 ℃; four sections: 260-275 ℃; five sections: 255-265 ℃; six sections: 255-265 ℃; seven sections: 245-260 ℃; eight sections: 245-260 ℃; nine sections: 245-260 ℃; ten sections: 245-260 ℃; the temperature of the machine head is 245-255 ℃; the six sections and the nine sections of the extruder are provided with vacuum devolatilizers;
the preparation method of the self-made flame-retardant master batch comprises the following steps:
mixing polycarbonate powder and methyl phenyl siloxane, adding a silsesquioxane flame retardant, potassium perfluorobutyl sulfonate, an antioxidant and a heat stabilizer, and mixing again;
uniformly mixing, adding into a double-screw extruder with the length-diameter ratio of 36:1, extruding, cooling the extruded material strips to room temperature through a water tank, and granulating; the temperature of each temperature zone of the twin-screw extruder is as follows: a section of: 235-245 ℃; two sections: 240-260 ℃; three sections: 250-265 ℃; four sections: 250-265 ℃; five sections: 250-265 ℃; six sections: 245-255 ℃; seven sections: 245-255 ℃; eight sections: 240-250 ℃; nine sections: 240-250 ℃; the temperature of the machine head is 240-250 ℃.
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