CN114395237A - Laser-engravable photodiffusion flame-retardant PC material and preparation method thereof - Google Patents
Laser-engravable photodiffusion flame-retardant PC material and preparation method thereof Download PDFInfo
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- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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-engravable light diffusion PC material which is characterized by comprising the following components in parts by mass: polycarbonate (C): 83-94 parts; photorefractive disruptor: 1-5 parts; self-made flame-retardant master batch: 2-10 parts; a toughening agent: 0.2-0.5 part; thermal stabilizer: 0.1-0.5 part; 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 etching auxiliary agent: 0.1-0.5 part; anti-dripping agent: 0.05 to 0.3 portion. The light diffusion PC with excellent flame retardant effect and good laser etching effect is obtained by adding a compound flame retardant system and a proper proportion of other materials and processing under a better process condition, 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-engravable light-diffusion flame-retardant PC material and a preparation method thereof.
Background
Along with the improvement of the requirements of people on living quality, the requirements on the appearance of plastic products related to life are higher and higher, the surface patterns of the traditional plastic products are generally manufactured by silk-screen printing, spraying and water transfer printing, 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, a computer is adopted to control and draw patterns, numbers, Chinese characters and the like, through data transmission, a laser etching technology utilizing a laser marking method is developed, light energy is converted into heat energy by adding a proper laser etching auxiliary agent, a pattern which is variable and multi-end and clear is obtained, time is saved, energy sources can be saved, and the laser etching technology is successfully applied to the fields of electronic appliances, livestock ear tags, cosmetic packages, automobile internal buttons and door handles, instrument panels, computer keyboards, glass lenses, medical devices and the like.
At present, plastic living products on the market are extremely diversified according to the application of PC, Polycarbonate (PC) has high chemical stability, certain flame retardant property, good heat resistance and transparency, notch sensitivity, poor hydrolysis resistance, poor organic chemical resistance, poor scratch resistance, poor weather resistance, yellowing after long-term exposure to ultraviolet rays, high-temperature use, high dimensional stability and good creep resistance, and in order to meet the use environment of the PC material used on a lamp, the PC material generally needs to ensure the light diffusion effect, the flame retardant effect, the good light transmittance and the aesthetic property, and additives such as flame retardants can be added into the PC material. In general, the fire retardant affects the transmittance and haze of polycarbonate, the transmittance of photodiffusion PC is higher, an infrared light source directly penetrates through the material, and a large amount of light energy cannot be converted into heat energy, so that the laser etching effect is difficult to obtain. And because of the occurrence of illumination, a little light energy is converted into heat energy and continuously accumulated 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 new type of photo-diffusible flame retardant PC material capable of laser etching is needed to solve the above problems.
The weather-resistant flame-retardant light diffusion PC material capable of being used for outdoor lamp shades is prepared from 81.25-90.17 wt% of PC, 5-15 wt% of a toughening agent, 0.8 wt% of a light diffusing agent, 1.5-2.5 wt% of a flame retardant, 0.4-0.6 wt% of a synergistic flame retardant, 0.1-0.5 wt% of a hydrolysis resistant agent, 0.1-0.5 wt% of an anti-UV agent, 0.03-0.05 wt% of a pigment, 0.3 wt% of an antioxidant and 0.3 wt% of a dispersant. 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, the fluorine-containing carbonate polyurethane elastomer is added as a toughening agent for modification, and the hydrolysis resistance agent and the light stabilizer are added to enable the color in the whole formula system to be yellow, so that the color is adjusted by using titanium dioxide and white carbon black with stronger covering power, and the whole formula system has better light diffusion and flame retardant effects.
The content of the flame retardant added into the material is less, and the material cannot be well dispersed, and because the titanium dioxide and the white carbon black with stronger covering power are added for adjusting the color, the transparency of the product is greatly reduced, the laser etching effect is influenced, and the product cannot obtain good appearance patterns.
Disclosure of Invention
The invention aims to provide a novel technical scheme of a laser-engravable light-diffusion flame-retardant PC material, so that the technical defects that the light diffusion is poor and laser engraving is difficult in the production and manufacturing process of flame-retardant PC in the prior art are overcome.
According to a first aspect of the invention, a laser-engravable light diffusion PC material is provided, which comprises the following components in parts by mass:
polycarbonate (C): 83-94 parts;
photorefractive disruptor: 1-5 parts;
self-made flame-retardant master batch: 2-10 parts;
a toughening agent: 0.2-0.5 part;
thermal stabilizer: 0.1-0.5 part;
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 etching auxiliary agent: 0.1-0.5 part;
anti-dripping agent: 0.05 to 0.3 portion.
Preferably, the composition comprises the following components in parts by weight:
polycarbonate (C): 92 parts of (1);
photorefractive disruptor: 2 parts of (1);
self-made flame-retardant master batch: 3.5 parts;
a toughening agent: 0.3 part;
thermal stabilizer: 0.3 part;
main antioxidant: 0.2 part;
auxiliary antioxidant: 0.2 part;
ultraviolet absorber: 0.15 part;
light diffusing agent: 0.8 part;
laser etching auxiliary agent: 0.2 part;
anti-dripping agent: 0.15.
preferably, the self-made flame-retardant master batch comprises the following components in parts by weight:
polycarbonate powder: 100 parts of (A);
potassium perfluorobutylsulfonate 2025: 5 parts of a mixture;
silsesquioxane flame retardant: 2 parts of (1);
methyl phenyl siloxane: 5 parts of a mixture;
thermal stabilizer: 1 part;
main antioxidant: 2 parts of (1);
auxiliary antioxidant: and 2 parts.
According to a second aspect of the present invention, there is provided a method for preparing the above laser-engravable light diffusion flame retardant PC material, which mainly comprises the following steps:
putting polycarbonate, a light refraction interference agent, self-made flame-retardant master batches, a toughening agent, an antioxidant, an ultraviolet absorbent, a light diffusant, an anti-dripping agent and a laser etching auxiliary agent into a high-speed mixer according to the mass parts for mixing;
adding the mixed materials into an extruder for extrusion;
and cooling the extruded material strips to room temperature through a water tank, and granulating through a granulator to complete the preparation of the laser-engravable light-diffusion flame-retardant PC material.
Preferably, the extruder is a double-screw extruder with a length-diameter ratio of 40:1, and the temperature of each temperature zone of the double-screw extruder is as follows: a first stage: 235-245 ℃; and (2) second stage: 260-275 ℃; and (3) three stages: 260-275 ℃; and a fourth stage: 260-275 ℃; five stages: 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;
uniformly mixing, adding the mixture 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 pelletizing.
Preferably, the temperature of each temperature zone of the twin-screw extruder is as follows: a first stage: 235-245 ℃; and (2) second stage: 240-260 ℃; and (3) three stages: 250 to 265 ℃; and a fourth stage: 250 to 265 ℃; five stages: 250 to 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 etching process, the material is carbonized by absorbing heat when black characters are etched, and the material is foamed when white characters are etched, so that the brominated flame retardant, the carbon black, the titanium dioxide and the white carbon black have a large influence on the laser etching effect in general, and a transparent product is transparent, so that the light energy can not be converted into heat energy, the laser etching auxiliary agent is added into the PC plastic product to help the PC plastic product to efficiently and uniformly absorb the laser energy, according to one embodiment of the patent disclosure, because the laser etching assistant is added into the material, under the action of laser beams, heating, carbonizing, evaporating and chemically reacting plastic, collecting energy, converting light energy into heat energy, improving laser etching effect, therefore, characters can be clearly and obviously etched, the laser etching speed and the color contrast are improved, and the original physical property of the plastic and the flame retardant effect after modification are not influenced.
The flame-retardant system used in the patent has small influence on the laser etching 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, and meanwhile, because the material does not contain bromine, the smoke generation amount and the toxic gas release amount can be greatly reduced during heating and burning, the environmental pollution is reduced, the material has low corrosivity on an injection mold, the processing cost is reduced, and the occurrence of suffocation caused by smoke of people can be reduced due to low VOC content during fire, so that the safety performance can be greatly improved;
this patent has used the compound fire-retardant system of perfluorobutyl potassium sulfonate, silsesquioxane and transparent methyl phenyl siloxane that the addition is still less, because it is reaction type flame retardant, the addition is few, has reduced the influence of flame retardant to radium carving effect. In addition, because the light transmittance of the transparent product is high, the light energy cannot be gathered, so that the light energy cannot be well converted into heat energy, and the transparent light diffusion PC cannot well engrave patterns even if a laser engraving aid 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, the laser engraving is facilitated, and the light source of the material is softer and brighter when the PC lampshade is produced. Meanwhile, laser etching assistant powder more suitable for transparent materials is added, so that a light diffusion flame-retardant PC material more suitable for laser etching is obtained;
the material utilizes perfluorobutyl potassium sulfonate 2025 as a main flame retardant, silsesquioxane QB-C02 and a methylphenylsiloxane reactive high-performance liquid additive as an auxiliary flame retardant for synergistic compounding, greatly improves the reduction of the 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, improves the Flame Retardance (FR) of polycarbonate, retains the high definition of minimum haze and hardly influences the transparency of the polycarbonate;
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 present invention will now be described in detail. It should be noted that: the relative arrangement of the components and steps, the numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless specifically stated otherwise.
The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses.
Techniques, methods, and apparatus known to those 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 particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values.
Example 1
A laser-engravable light diffusion PC material comprises the following components in parts by mass:
polycarbonate (C): 83-94 parts;
photorefractive disruptor: 1-5 parts;
self-made flame-retardant master batch: 2-10 parts;
a toughening agent: 0.2-0.5 part;
thermal stabilizer: 0.1-0.5 part;
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 etching auxiliary agent: 0.1-0.5 part;
anti-dripping agent: 0.05-0.3.
The self-made flame-retardant master batch in the embodiment comprises the following components in parts by weight:
polycarbonate powder: 100 parts of (A);
potassium perfluorobutylsulfonate 2025: 5 parts of a mixture;
silsesquioxane QB-C02: 2 parts of (1);
methyl phenyl siloxane: 5 parts of a mixture;
thermal stabilizer: 1 part;
main antioxidant: 2 parts of (1);
auxiliary antioxidant: and 2 parts.
Wherein the polycarbonate is high-viscosity polycarbonate PC 110; the photorefractive interference agent is ABS 920; the toughening agent is maleic anhydride modified polyethylene wax 1105A; the heat stabilizer is C-10 RW; the main antioxidant of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid octadecyl ester is 1076; the phosphite ester auxiliary antioxidant is 168; the high molecular weight hydroxyphenyl benzotriazole ultraviolet light absorber is UV-234; the Japanese ponding light diffusant is EXM-5; the laser etching auxiliary agent is Merck 8825; the anti-dripping agent is Polytetrafluoroethylene (PTFE).
Under the condition that a micromolecular lubricant with the function of promoting degradation is not additionally added, the PC is modified by using the wax transparent dispersion toughening agent with a macromolecular chain, the addition amount is small, the transparency and haze of a product are not influenced, the good self-lubricating function can ensure that the flame-retardant master batch and other additives can obtain a better dispersion effect in a screw rod while toughening, so that a good flame-retardant polycarbonate product resistant to environmental stress cracking can be obtained, particularly for the product of a screw insert, the phenomenon of stress concentration can be weakened, and the periphery of the screw can not crack due to over-concentrated stress;
the powdery heat stabilizer C-10RW which is low in volatility and not easy to hydrolyze and is produced by using the high-molecular-weight hydroxyphenyl benzotriazole ultraviolet absorbent with low volatility, strong light absorption and good compatibility with base materials and the new dry material is synergistic and is used stably, so that the light aging resistance is good, and the yellowing resistance is realized under outdoor conditions. The heat stabilizer can effectively resist the degradation, yellowing and fading of the polymer caused by shearing and hot pressure in the processing process, and simultaneously, the heat stabilizer and the antioxidant are used as a synergistic heat stabilizer, so that the performance of the end group is more stable, the depolymerization at high temperature is not easy to occur, and the service life of the polymer is prolonged under the condition of heat aging. Due to the addition of the two suitable light and heat aging system products, the surface is not yellowed and precipitated after long-term use, and the long-term use of the product is not influenced.
The flame-retardant system in the patent is a flame-retardant composite system of perfluorobutyl potassium sulfonate 2025, silsesquioxane QB-C02 and methylphenylsiloxane. The product produced by the flame-retardant system does not affect the transparency, and the heat resistance of the material is higher, except for adding the reactive potassium perfluorobutylsulfonate, the synergistic effect of the silsesquioxane, the methylphenylsiloxane and the main flame-retardant system is utilized, so that the better flame-retardant photodiffusion PC capable of laser engraving is obtained.
Because the addition amount of the flame retardant is less, in order to uniformly disperse the flame retardant, the powdery polycarbonate and the flame retardant are mixed more easily, and the obtained flame-retardant master batch has better dispersion effect, so that the flame retardant is prepared into particles in advance and then added, and is more easily and uniformly dispersed.
Because the fire retardant has an influence on the laser etching powder, the addition of the fire retardant can disperse energy instantly, the laser etching auxiliary agent can gather energy, the influence of the brominated fire retardant on the laser etching is larger, the reaction type fire retardant without bromine and chlorine has a smaller influence on the laser etching effect, and the smaller the addition 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 a light source is reduced quickly, and after the brominated flame retardant is added with the laser etching powder, etching is not easy to occur, and characters are not clear. Therefore, the traditional method for producing transparent polycarbonate by modifying Polycarbonate (PC) with brominated flame retardant is changed in the embodiment, the bromine-free and chlorine-free flame retardant is used, the light source is better dispersed, and the product has better laser etching effect.
The preparation method of the laser-engravable light-diffusion flame-retardant PC material in the embodiment mainly comprises the following steps:
putting polycarbonate, a light refraction interference agent ABS920, self-made flame-retardant master batches, a toughening agent, an antioxidant, an ultraviolet absorbent, a light diffusant, an anti-dripping agent and a laser etching auxiliary agent into a high-speed mixer according to the mass parts, uniformly mixing for 3 minutes, adding the uniformly mixed materials into an extruder, and extruding; and cooling the extruded material strips to room temperature through a water tank, and granulating through a granulator to complete the preparation of the laser-engravable light-diffusion flame-retardant PC material.
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 first stage: 235-245 ℃; and (2) second stage: 260-275 ℃; and (3) three stages: 260-275 ℃; and a fourth stage: 260-275 ℃; five stages: 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 plastic, and is sensitive to shearing heat, in order to reduce the generation of shearing heat, the processing temperature of a melting section from a feed opening to four regions is set to be high-temperature processed, so that the polycarbonate material can be quickly melted in a double-screw extruder, the shearing heat of the double-screw extruder to the material is reduced, the torque of a screw is reduced, the loss of equipment is further reduced, meanwhile, good dispersion can be carried out in the shearing section, the processing temperature of the shearing and dispersing section is reduced, and the degradation of the polycarbonate material is reduced.
And the six sections and the nine sections of the extruder are provided with vacuum devolatilizers to realize double vacuum control, so that the odor of the modified product and the volatilization of harmful substances thereof are improved and controlled.
Before production, the polycarbonate needs to be dried at 120 ℃ for 4-6 hours, after the materials are mixed, the sealing is required to be carried out, the materials are used as soon as possible, the polycarbonate is prevented from absorbing moisture again, after the materials are granulated, the materials are cooled by water at 40 ℃ and then are separated from water, and the hydrolysis phenomenon in the production process is prevented from affecting the performance of the materials.
The preparation method of the self-made flame-retardant master batch in the embodiment comprises the following steps:
uniformly mixing polycarbonate powder and methyl phenyl siloxane (liquid) for 2 minutes, uniformly adding a flame retardant of potassium perfluorobutylsulfonate, a silsesquioxane flame retardant, an antioxidant and a heat stabilizer in parts by weight into the mixed polycarbonate, and uniformly mixing for 2 minutes again; uniformly mixing, adding the mixture 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 pelletizing.
Wherein the temperature of each temperature zone of the double-screw extruder is as follows: a first stage: 235-245 ℃; and (2) second stage: 240-260 ℃; and (3) three stages: 250 to 265 ℃; and a fourth stage: 250 to 265 ℃; five stages: 250 to 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 influence on the material performance caused by the thermal degradation of the self-made flame-retardant master batch due to the shearing heat of the double-screw extruder, the double-screw extruder with the length-diameter ratio of 36:1 is used, and simultaneously, because the methylphenylsiloxane is liquid and is volatile at high temperature, the low-temperature processing with gradual temperature rise is used in a first area and a second area of a feed opening to reduce the volatilization of the liquid flame-retardant synergist, so that the rapid temperature rise is carried out in three to five areas to rapidly melt the polycarbonate material, and the dispersion of the flame retardant in the double-screw extruder is accelerated. After the dispersing of various auxiliary materials is finished, the materials are extruded at a low temperature at a machine head, so that the thermal degradation of the materials is reduced, and excellent physical and chemical properties are preserved for secondary processing.
Example 2
The laser-engravable light diffusion PC material comprises the following components in parts by mass:
polycarbonate (C): 83 parts of a solvent;
photorefractive disruptor: 5 parts of a mixture;
self-made flame-retardant master batch: 10 parts of (A);
a toughening agent: 0.2 part;
thermal stabilizer: 0.1 part;
main antioxidant: 0.1 part;
auxiliary antioxidant: 0.3 part;
ultraviolet absorber: 0.4 part;
light diffusing agent: 0.5 part;
laser etching auxiliary agent: 0.1 part;
anti-dripping agent: 0.3 part.
Wherein the polycarbonate is high-viscosity polycarbonate PC 110; the photorefractive interference agent is ABS 920; the toughening agent is maleic anhydride modified polyethylene wax 1105A; the heat stabilizer is C-10 RW; the main antioxidant of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid octadecyl ester is 1076; the phosphite ester auxiliary antioxidant is 168; the high molecular weight hydroxyphenyl benzotriazole ultraviolet light absorber is UV-234; the Japanese ponding light diffusion is EXM-5; the laser etching auxiliary agent is Merck 8825; the anti-dripping agent is Polytetrafluoroethylene (PTFE).
The flame-retardant master batch in the embodiment comprises the following components in parts by weight:
polycarbonate powder: 100 parts of (A);
potassium perfluorobutylsulfonate 2025: 5 parts of a mixture;
silsesquioxane QB-C02: 2 parts of (1);
methyl phenyl siloxane: 5 parts of a mixture;
thermal stabilizer: 1 part;
main antioxidant: 2 parts of (1);
auxiliary antioxidant: and 2 parts.
Wherein the flame-retardant system is a flame-retardant composite system of potassium perfluorobutylsulfonate 2025, silsesquioxane QB-C02 and methylphenylsiloxane. Experimental parts were prepared according to the preparation method in example 1.
Example 3
A laser-engravable light diffusion PC material comprises the following components in parts by mass:
polycarbonate (C): 94 parts of a binder;
photorefractive disruptor: 1 part;
self-made flame-retardant master batch: 2 parts of (1);
a toughening agent: 0.5 part;
thermal stabilizer: 0.5 part;
main antioxidant: 0.3 part;
auxiliary antioxidant: 0.1 part;
ultraviolet absorber: 0.1 part;
light diffusing agent: 1 part;
laser etching auxiliary agent: 0.5 part;
anti-dripping agent: 0.05 part.
Wherein the polycarbonate is high-viscosity polycarbonate PC 110; the photorefractive interference agent is ABS 920; the toughening agent is maleic anhydride modified polyethylene wax 1105A; the heat stabilizer is C-10 RW; the main antioxidant of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid octadecyl ester is 1076; the phosphite ester auxiliary antioxidant is 168; the high molecular weight hydroxyphenyl benzotriazole ultraviolet light absorber is UV-234; the Japanese ponding light diffusion is EXM-5; the merck laser etching auxiliary agent is 8825; the anti-dripping agent is Polytetrafluoroethylene (PTFE).
The self-made flame-retardant master batch in the embodiment comprises the following components in parts by weight:
polycarbonate powder: 100 parts of (A);
potassium perfluorobutylsulfonate 2025: 5 parts of a mixture;
silsesquioxane QB-C02: 2 parts of (1);
methyl phenyl siloxane: 5 parts of a mixture;
thermal stabilizer: 1 part;
main antioxidant: 2 parts of (1);
auxiliary antioxidant: and 2 parts.
Wherein the flame-retardant system is a flame-retardant composite system of potassium perfluorobutylsulfonate 2025, silsesquioxane QB-C02 and methylphenylsiloxane. Experimental parts were prepared according to the preparation method in example 1.
Example 4
A laser-engravable light diffusion PC material comprises the following components in parts by mass:
polycarbonate (C): 92 parts of (1);
photorefractive disruptor: 2 parts of (1);
self-made flame-retardant master batch: 3.5 parts;
a toughening agent: 0.3 part;
thermal stabilizer: 0.3 part;
main antioxidant: 0.2 part;
auxiliary antioxidant: 0.2 part;
ultraviolet absorber: 0.15 part;
light diffusing agent: 0.8 part;
laser etching auxiliary agent: 0.2 part;
anti-dripping agent: 0.15 part.
Wherein the polycarbonate is high-viscosity polycarbonate PC 110; the photorefractive interference agent is ABS 920; the toughening agent is maleic anhydride modified polyethylene wax 1105A; the heat stabilizer is C-10 RW; the main antioxidant of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid octadecyl ester is 1076; the phosphite ester auxiliary antioxidant is 168; the high molecular weight hydroxyphenyl benzotriazole ultraviolet light absorber is UV-234; the Japanese ponding light diffusion is EXM-5; the merck laser etching auxiliary agent is 8825; the anti-dripping agent is Polytetrafluoroethylene (PTFE).
The self-made flame-retardant master batch in the embodiment comprises the following components in parts by weight:
polycarbonate powder: 100 parts of (A);
potassium perfluorobutylsulfonate 2025: 5 parts of a mixture;
silsesquioxane QB-C02: 2 parts of (1);
methyl phenyl siloxane: 5 parts of a mixture;
thermal stabilizer: 1 part;
main antioxidant: 2 parts of (1);
auxiliary antioxidant: and 2 parts.
Wherein the flame-retardant system is a flame-retardant composite system of potassium perfluorobutylsulfonate 2025, silsesquioxane QB-C02 and methylphenylsiloxane. The self-made flame retardant masterbatch was prepared according to the preparation method in example 1.
Comparative example 1
A laser-engravable light diffusion PC material comprises the following components in parts by mass:
polycarbonate (C): 92 parts of (1);
photorefractive disruptor: 2 parts of (1);
self-made flame-retardant master batch: 3.5 parts;
a toughening agent: 0.3 part;
thermal stabilizer: 0.3 part;
main antioxidant: 0.2 part;
auxiliary antioxidant: 0.2 part;
ultraviolet absorber: 0.15 part;
light diffusing agent: 0.8 part;
laser etching auxiliary agent: 0.2 part;
anti-dripping agent: 0.15 part.
Titanium dioxide: 1 part of
Wherein the polycarbonate is high-viscosity polycarbonate PC 110; the photorefractive interference agent is ABS 920; the toughening agent is maleic anhydride modified polyethylene wax 1105A; the heat stabilizer is C-10 RW; the main antioxidant of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid octadecyl ester is 1076; the phosphite ester auxiliary antioxidant is 168; the high molecular weight hydroxyphenyl benzotriazole ultraviolet light absorber is UV-234; the Japanese ponding light diffusion is EXM-5; the merck laser etching auxiliary agent is 8825; the anti-dripping agent is Polytetrafluoroethylene (PTFE); the titanium dioxide is DuPont R105.
The self-made flame-retardant master batch in the embodiment comprises the following components in parts by weight:
polycarbonate powder: 100 parts of (A);
potassium perfluorobutylsulfonate 2025: 5 parts of a mixture;
silsesquioxane QB-C02: 2 parts of (1);
methyl phenyl siloxane: 5 parts of a mixture;
thermal stabilizer: 1 part;
main antioxidant: 2 parts of (1);
auxiliary antioxidant: and 2 parts.
Wherein the flame-retardant system is a flame-retardant composite system of potassium perfluorobutylsulfonate 2025, silsesquioxane QB-C02 and methylphenylsiloxane. The self-made flame retardant masterbatch was prepared according to the preparation method in example 1.
Comparative example 2
A laser-engravable light diffusion PC material comprises the following components in parts by mass:
polycarbonate (C): 94 parts of a binder;
self-made flame-retardant master batch: 3.5 parts;
a toughening agent: 0.3 part;
thermal stabilizer: 0.3 part;
main antioxidant: 0.2 part;
auxiliary antioxidant: 0.2 part;
ultraviolet absorber: 0.15 part;
light diffusing agent: 0.8 part;
laser etching auxiliary agent: 0.2 part;
anti-dripping agent: 0.15 part.
Wherein the polycarbonate is high-viscosity polycarbonate PC 110; the toughening agent is maleic anhydride modified polyethylene wax 1105A; the heat stabilizer is C-10 RW; the main antioxidant of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid octadecyl ester is 1076; the phosphite ester auxiliary antioxidant is 168; the high molecular weight hydroxyphenyl benzotriazole ultraviolet light absorber is UV-234; the Japanese ponding light diffusant is EXM-5; the laser etching auxiliary agent is Merck 8825; the anti-dripping agent is Polytetrafluoroethylene (PTFE).
The material is prepared by the whole formula under the condition of not adding a photorefractive interference agent, namely ABS 920.
The self-made flame-retardant master batch in the embodiment comprises the following components in parts by weight:
polycarbonate powder: 100 parts of (A);
potassium perfluorobutylsulfonate 2025: 5 parts of a mixture;
silsesquioxane QB-C02: 2 parts of (1);
methyl phenyl siloxane: 5 parts of a mixture;
thermal stabilizer: 1 part;
main antioxidant: 2 parts of (1);
auxiliary antioxidant: and 2 parts.
Wherein the flame-retardant system is a flame-retardant composite system of potassium perfluorobutylsulfonate 2025, silsesquioxane QB-C02 and methylphenylsiloxane. Experimental parts were prepared according to the preparation method in example 1.
Comparative example 3
A laser-engravable light diffusion PC material comprises the following components in parts by mass:
polycarbonate (C): 87 parts of a mixture;
photorefractive disruptor: 2 portions of
Self-made flame-retardant master batch: 10 parts of (A);
a toughening agent: 0.3 part;
thermal stabilizer: 0.3 part;
main antioxidant: 0.2 part;
auxiliary antioxidant: 0.2 part;
ultraviolet absorber: 0.15 part;
light diffusing agent: 0.8 part;
laser etching auxiliary agent: 0.2 part;
anti-dripping agent: 0.15 part.
Wherein the polycarbonate is high-viscosity polycarbonate PC 110; the photorefractive interference agent is ABS 920; the toughening agent is maleic anhydride modified polyethylene wax 1105A; the heat stabilizer is C-10 RW; the main antioxidant of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid octadecyl ester is 1076; the phosphite ester auxiliary antioxidant is 168; the high molecular weight hydroxyphenyl benzotriazole ultraviolet light absorber is UV-234; the Japanese ponding light diffusion is EXM-5; the merck laser etching auxiliary agent is 8825; the anti-dripping agent is Polytetrafluoroethylene (PTFE).
The self-made flame-retardant master batch in the embodiment comprises the following components in parts by weight:
polycarbonate powder: 100 parts of (A);
bisphenol a bis (diphenyl phosphate) (BDP): 35 parts of (B);
potassium perfluorobutylsulfonate 2025: 5 parts of a mixture;
thermal stabilizer: 1 part;
main antioxidant: 2 parts of (1);
auxiliary antioxidant: and 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 five zones by a side-fed liquid metering device (hydraulic pressure).
And 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 pelletizing.
Preferably, the temperature of each temperature zone of the twin-screw extruder is as follows: a first stage: a first stage: 235-245 ℃; and (2) second stage: 260-275 ℃; and (3) three stages: 260-275 ℃; and a fourth stage: 260-275 ℃; five stages: 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 adopts that one to four areas are quickly melted 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 feeding inlet of the five sections of liquid, the BDP is prevented from being added at high temperature to increase the degradation degree, and the loss of the BDP is increased in the vaporization process.
Comparative example 4
A laser-engravable light diffusion PC material comprises the following components in parts by mass:
polycarbonate (C): 87 parts of a mixture;
photorefractive disruptor: 2 portions of
Self-made flame-retardant master batch: 10 parts of (A);
a toughening agent: 0.3 part;
thermal stabilizer: 0.3 part;
main antioxidant: 0.2 part;
auxiliary antioxidant: 0.2 part;
ultraviolet absorber: 0.15 part;
light diffusing agent: 0.8 part;
laser etching auxiliary agent: 0.2 part;
anti-dripping agent: 0.15 part.
Wherein the polycarbonate is high-viscosity polycarbonate PC 110; the photorefractive interference agent is ABS 920; the toughening agent is maleic anhydride modified polyethylene wax 1105A; the heat stabilizer is C-10 RW; the main antioxidant of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid octadecyl ester is 1076; the phosphite ester auxiliary antioxidant is 168; the high molecular weight hydroxyphenyl benzotriazole ultraviolet light absorber is UV-234; the Japanese ponding light diffusion is EXM-5; the merck laser etching auxiliary agent is 8825; the anti-dripping agent is Polytetrafluoroethylene (PTFE).
The flame-retardant master batch in the embodiment comprises the following components in parts by weight:
polycarbonate powder: 100 parts of (A);
bromo triazine (245): 70 parts of (B);
thermal stabilizer: 1 part;
main antioxidant: 2 parts of (1);
auxiliary antioxidant: and 2 parts.
Wherein the flame retardant system is a brominated triazine single brominated system. Preferably, the preparation method of the flame-retardant master batch comprises the following steps:
mixing polycarbonate powder, bromotriazine, an antioxidant and a heat stabilizer; uniformly mixing, adding the mixture 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 pelletizing.
Preferably, the temperature of each temperature zone of the twin-screw extruder is as follows: a first stage: a first stage: 235-245 ℃; and (2) second stage: 260-275 ℃; and (3) three stages: 260-275 ℃; and a fourth stage: 260-275 ℃; five stages: 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 adopts high-temperature melting materials used in the first half section, so that the dispersion of the shearing section is accelerated, and the normal production is carried out according to the conventional process after five sections, so that the thermal degradation of the materials is reduced.
Comparative example 5
A laser-engravable light diffusion PC material comprises the following components in parts by mass:
polycarbonate (C): 94 parts of a binder;
photorefractive disruptor: 2 portions of
Self-made flame-retardant master batch: 3.5 parts;
a toughening agent: 0.3 part;
thermal stabilizer: 0.3 part;
main antioxidant: 0.2 part;
auxiliary antioxidant: 0.2 part;
ultraviolet absorber: 0.15 part;
light diffusing agent: 0.8 part;
laser etching auxiliary agent: 0.2 part;
anti-dripping agent: 0.15 part.
Wherein the polycarbonate is high-viscosity polycarbonate PC 110; the photorefractive interference agent is ABS 920; the toughening agent is maleic anhydride modified polyethylene wax 1105A; the heat stabilizer is C-10 RW; the main antioxidant of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid octadecyl ester is 1076; the phosphite ester auxiliary antioxidant is 168; the high molecular weight hydroxyphenyl benzotriazole ultraviolet light absorber is UV-234; the Japanese ponding light diffusion is EXM-5; the laser carving auxiliary agent is changed into a domestic model; the anti-dripping agent is Polytetrafluoroethylene (PTFE).
The self-made flame-retardant master batch in the embodiment comprises the following components in parts by weight:
polycarbonate powder: 100 parts of (A);
potassium perfluorobutylsulfonate 2025: 5 parts of a mixture;
silsesquioxane QB-C02: 2 parts of (1);
methyl phenyl siloxane: 5 parts of a mixture;
thermal stabilizer: 1 part;
main antioxidant: 2 parts of (1);
auxiliary antioxidant: and 2 parts.
Wherein the flame-retardant system is a flame-retardant composite system of potassium perfluorobutylsulfonate 2025, silsesquioxane QB-C02 and methylphenylsiloxane. Experimental parts were prepared according to the preparation method in example 1.
Comparative example 6
A laser-engravable light diffusion PC material comprises the following components in parts by mass:
polycarbonate (C): 91 parts of;
photorefractive disruptor: 2 portions of
Self-made flame-retardant master batch: 3.5 parts;
a toughening agent: 3 parts of a mixture;
thermal stabilizer: 0.3 part;
main antioxidant: 0.2 part;
auxiliary antioxidant: 0.2 part;
ultraviolet absorber: 0.15 part;
light diffusing agent: 0.8 part;
laser etching auxiliary agent: 0.2 part;
anti-dripping agent: 0.15 part.
Wherein the polycarbonate is high-viscosity polycarbonate PC 110; the photorefractive interference agent is ABS 920; the toughening agent is polymethyl methacrylate-butadiene-styrene terpolymer (MBS); the heat stabilizer is C-10 RW; the main antioxidant of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid octadecyl ester is 1076; the phosphite ester auxiliary antioxidant is 168; the high molecular weight hydroxyphenyl benzotriazole ultraviolet light absorber is UV-234; the Japanese ponding light diffusion is EXM-5; the merck laser etching auxiliary agent is 8825; the anti-dripping agent is Polytetrafluoroethylene (PTFE).
The self-made flame-retardant master batch in the embodiment comprises the following components in parts by weight:
polycarbonate powder: 100 parts of (A);
potassium perfluorobutylsulfonate 2025: 5 parts of a mixture;
silsesquioxane QB-C02: 2 parts of (1);
methyl phenyl siloxane: 5 parts of a mixture;
thermal stabilizer: 1 part;
main antioxidant: 2 parts of (1);
auxiliary antioxidant: and 2 parts.
Wherein the flame-retardant system is a flame-retardant composite system of potassium perfluorobutylsulfonate 2025, silsesquioxane QB-C02 and methylphenylsiloxane. Experimental parts were prepared according to the preparation method in example 1.
The experimental parts of examples 2 to 4 were compared with the experimental parts of comparative examples 1 to 6, and the results of comparison in terms of melt flow rate, elongation at break, notched izod impact strength, glow wire, 1.4mm haze, 1.4mm light transmittance, xenon lamp radiation exposure, flame retardant effect, appearance color, laser etching effect, etc., are shown in table 1
Table 1 comparison of the parameters of the experimental materials of examples 2 to 4 with those of comparative examples 1 to 6
Relevant test methods and standards:
1. melt flow rate: GB/T1033;
2. elongation at break: ISO 527;
3. the notched impact strength of the cantilever beam is GB/T1843
4. Glow wire: IEC 60695-2-12;
5. haze ASTM D-1003-2007;
6. total light transmittance: DIN 5036-1;
7. flame retardant UL 94-2006;
8. xenon lamp artificial weathering test, method for testing light source in plastics laboratories section two: xenon arc lamps GB/T16422.2-1999;
9. laser etching test: the laser has clear and sharp marks, high speed and high contrast for 1060nm near-infrared laser.
It can be seen from the data in the table that in the example 2 and the example 3, the former has more influence due to the added self-made flame retardant master batch and the ABS photo-interference agent, although the flame retardant property of the material is better, the product surface is white, the light source is yellowish, the flame retardant influences the laser etching effect, the laser etching agent is less, the overall laser etching effect is not very good, and the light diffusion effect in the example 2 is worse than that in the example 3. In example 4, the auxiliary materials are suitable in proportion, the product has moderate surface transmittance and haze, a soft light source, high physical properties, a good laser etching effect, high impact strength, good weather resistance, a high glowing filament service temperature and a good light diffusion effect. In the comparative example 1, 1 part of titanium dioxide is added on the basis of the example 4, the melt flow rate, the elongation at break and the impact strength are reduced, the transmittance is reduced, the haze is larger, the light source is white, and due to the introduction of the titanium dioxide, the self covering capability is stronger, the light diffusion effect of the material is weaker than that of the example 4, the material becomes worse, and the laser etching effect is worse. In comparative example 2, ABS with light interference effect is not added, so that even if a light stabilizer is added to the material, the surface of the product is provided with light-transmitting beads, and the light source is not soft enough and has enough brightness in the daily use process, but the material is dazzling when being directly watched. And because the transparency is too high, the light source transmittance is too high, light energy cannot be converted into heat energy, the laser etching effect is poor, and the light diffusion effect is poor. In comparative example 3, the liquid flame retardant is added, so that the efficiency of the reactive flame retardant is higher than that of the sulfonate, the potassium perfluorobutylsulfonate and the silsesquioxane, the addition amount is larger, the thermal deformation temperature and the service temperature of the glow wire of the material are greatly influenced, the larger the addition amount is, the lower the impact strength is, the poorer the heat resistance is, the light diffusion effect is good, and the laser etching effect is general. In the comparative example 4, because a brominated flame retardant system is used, the impact strength of the whole material is greatly influenced, and because the flame retardant efficiency of the flame retardant is lower than that of flame retardants such as sulfonate, potassium perfluorobutane sulfonate, silsesquioxane and the like, the flame retardant effect is poor, because the influence of the brominated flame retardant on the laser etching effect is large, the laser etching effect is poor, and the service temperature of the glow wire is low. The light diffusion effect is poor, the transmittance and the haze are poor, the light source is soft, the color is easy to change during high-temperature processing, and the light diffusion effect is poor. The comparison column 5 uses the domestic laser etching powder, the laser etching powder is transparent light yellow powder, the product has moderate transmittance and haze, the surface is yellow, the light source is warm, the laser etching effect is poor, and the light diffusion effect is good. In the comparison column 6, the transparency and haze of the product are affected due to the use of the toughening agent of the polymethyl methacrylate-butadiene-styrene terpolymer (MBS), and the product is low in transparency, high in haze and slightly weak in diffusion effect because the rubber content is too high, the product is not easy to disperse in a formula system, the dispersion requirement on a screw rod in a processing process is higher, and the product is low in transparency, high in haze and slightly weak in diffusion effect.
Although some specific embodiments of the present invention have been described in detail by way of examples, it should be understood by those skilled in the art that the above examples are for illustrative purposes only and are not intended to limit the scope of the present 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 (7)
1. The laser-engravable light diffusion PC material is characterized by comprising the following components in parts by mass:
polycarbonate (C): 83-94 parts;
photorefractive disruptor: 1-5 parts;
self-made flame-retardant master batch: 2-10 parts;
a toughening agent: 0.2-0.5 part;
thermal stabilizer: 0.1-0.5 part;
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 etching auxiliary agent: 0.1-0.5 part;
anti-dripping agent: 0.05 to 0.3 portion.
2. The laser-engravable light diffusion PC material according to claim 1, comprising the following components in parts by mass:
polycarbonate (C): 92 parts of (1);
photorefractive disruptor: 2 parts of (1);
self-made flame-retardant master batch: 3.5 parts;
a toughening agent: 0.3 part;
thermal stabilizer: 0.3 part;
main antioxidant: 0.2 part;
auxiliary antioxidant: 0.2 part;
ultraviolet absorber: 0.15 part;
light diffusing agent: 0.8 part;
laser etching auxiliary agent: 0.2 part;
anti-dripping agent: 0.15.
3. the laser-engravable light diffusion PC material according to claim 1 or 2, wherein the self-made flame-retardant master batch comprises the following components in parts by weight:
polycarbonate powder: 100 parts of (A);
potassium perfluorobutylsulfonate 2025: 5 parts of a mixture;
silsesquioxane flame retardant: 2 parts of (1);
methyl phenyl siloxane: 5 parts of a mixture;
thermal stabilizer: 1 part;
main antioxidant: 2 parts of (1);
auxiliary antioxidant: and 2 parts.
4. A method for preparing the laser-engravable light diffusion flame-retardant PC material as claimed in any one of the claims 1 to 3, which is characterized by mainly comprising the following steps:
putting polycarbonate, a light refraction interference agent, self-made flame-retardant master batches, a toughening agent, an antioxidant, an ultraviolet absorbent, a light diffusant, an anti-dripping agent and a laser etching auxiliary agent into a high-speed mixer according to the mass parts for mixing;
adding the mixed materials into an extruder for extrusion;
and cooling the extruded material strips to room temperature through a water tank, and granulating through a granulator to complete the preparation of the laser-engravable light-diffusion flame-retardant PC material.
5. The method for preparing the laser-engravable light-diffusion flame-retardant PC material according to claim 4, wherein the extruder is a double-screw extruder with a length-diameter ratio of 40:1, and the temperature of each temperature zone of the double-screw extruder is as follows: a first stage: 235-245 ℃; and (2) second stage: 260-275 ℃; and (3) three stages: 260-275 ℃; and a fourth stage: 260-275 ℃; five stages: 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.
6. The preparation method of the laser-engravable light-diffusion flame-retardant PC material according to claim 5, wherein the preparation method of the self-made flame-retardant master batch is as follows:
mixing polycarbonate powder and methyl phenyl siloxane, adding a silsesquioxane flame retardant, potassium perfluorobutyl sulfonate, an antioxidant and a heat stabilizer, and then mixing again;
uniformly mixing, adding the mixture 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 pelletizing.
7. The method for preparing the laser-engravable light-diffusion flame-retardant PC material according to claim 6, wherein the temperature of each temperature zone of the double-screw extruder is as follows: a first stage: 235-245 ℃; and (2) second stage: 240-260 ℃; and (3) three stages: 250 to 265 ℃; and a fourth stage: 250 to 265 ℃; five stages: 250 to 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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| CN115991930A (en) * | 2022-11-30 | 2023-04-21 | 惠州市沃特新材料有限公司 | Polycarbonate composite material and preparation method and application thereof |
| CN115991930B (en) * | 2022-11-30 | 2024-06-07 | 惠州市沃特新材料有限公司 | Polycarbonate composite material and preparation method and application thereof |
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