CN102702716A - High light-transmittance and high flame-retardant polycarbonate material and preparation method of polycarbonate material - Google Patents

High light-transmittance and high flame-retardant polycarbonate material and preparation method of polycarbonate material Download PDF

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Publication number
CN102702716A
CN102702716A CN2012102211934A CN201210221193A CN102702716A CN 102702716 A CN102702716 A CN 102702716A CN 2012102211934 A CN2012102211934 A CN 2012102211934A CN 201210221193 A CN201210221193 A CN 201210221193A CN 102702716 A CN102702716 A CN 102702716A
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China
Prior art keywords
polycarbonate
inhibitor
fire retardant
flame retardant
transmission rate
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CN2012102211934A
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CN102702716B (en
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邓虎
傅轶
李文波
招启强
谭颂斌
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Guangdong Silverage Holdings Ltd.
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DONGGUAN YINXI PHOTOELECTRIC MATERIAL TECHNOLOGY CO LTD
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/04—Particle-shaped
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/78—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling
    • B29C48/875—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling for achieving a non-uniform temperature distribution, e.g. using barrels having both cooling and heating zones
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/92—Measuring, controlling or regulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/92514—Pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/92704—Temperature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92819—Location or phase of control
    • B29C2948/92857—Extrusion unit
    • B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/92895—Barrel or housing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92819—Location or phase of control
    • B29C2948/92857—Extrusion unit
    • B29C2948/92904—Die; Nozzle zone

Abstract

The invention relates to the technical field of polycarbonate material, particularly to high light-transmittance and high flame-retardant polycarbonate material. The polycarbonate material contains the following constituents and materials by weight: 94.8-99.5% of polycarbonate, 0.1-0.3% of fire retardant A, 0.1-3.5% of fire retardant B, 0.1-0.3% of antioxidant A, 0.1-0.3% of antioxidant B, 0.1-0.2% of a lubricating agent and 0-0.6% of light stabilizer, and the sum of the weight percentages of the constituents is 100%. The preparation method comprises the steps of putting the constituents except for the polycarbonate into a high-speed mixer to uniformly agitate, putting the polycarbonate and uniformly mixed material into the high-speed mixer to carry out three-segment agitation, and putting the material into a double-screw extruder to extrude and pelletize. The polycarbonate material disclosed by the invention has the advantages of high light transmittance and high fire resistance and the like, can meet the requirements of a lampshade for outdoor illumination, and is simple in process and beneficial for generalization and application.

Description

A kind of high transmission rate, high flame retardant polycarbonate material and preparation method thereof
Technical field
The present invention relates to the polycarbonate material technical field, particularly a kind of high transmission rate, high flame retardant polycarbonate material and preparation method thereof.
Background technology
Photodiode (Light Emitting Diode; LED) plurality of advantages such as energy-conserving and environment-protective characteristic little because of its volume, that the life-span is grown, colour developing is abundant and outstanding obtain increasingly extensive application in fields such as demonstration, traffic, electrical equipment and illuminations, are one of gordian techniquies of China's energy-saving and emission-reduction, cleaner production and Sustainable development.
LED is because the characteristics of luminescence of its pointolite, and lighting area is little, brightness of illumination is low etc. with respect to the weak point of conventional light source being applied to exist on the lighting field.For remedying the deficiency that led light source is used on lighting field, need change the characteristics of luminescence of its pointolite into area source through exotic materials, keep higher transmittance simultaneously.
Polycarbonate material is selected for use to be the lighting outer cover material owing to its intensity height, the transparency, high thermal resistance and flame retardant resistance usually.When the polycarbonate of non-modified is used as the light fixture outer cover; Flame retardant properties is lower; Need carry out special flame-retardant modified with protection LED lamp source, prevent that the lamp source is destroyed or receives sun exposure and variable color, yet as LED outdoor lighting lamp outer cover the time, the polycarbonate outer cover can cause transmittance to descend through traditional after flame-retardant modified; There is the low problem of luminous efficiency, can't brings into play the characteristics of LED illumination high brightness.
One Chinese patent application number is 2011110151541.0 patent of invention, has announced a kind of LED light fixture with fire-retardant light diffusing polycarbonate resin composite materials and preparation method thereof, comprises the component that following mass percent is formed: polycarbonate resin 75-90%; Brominated polycarbonate 5-10%; Organic silicon fibre retardant 2-5%, light diffusing agent 0.5-8%, thermo-stabilizer 0.1-0.5%; Photostabilizer 0.1-0.5%, processing aid 0-1%.Yet there is following shortcoming in this documents: 1, the large usage quantity of main flame retardant, and the shock resistance of the polycarbonate material that makes is relatively poor; Only can reach the IZOD notched Izod impact strength of 100-200, cracked easily during the product assembling, in addition; Cause the easy flavescence of product later stage, quality product descends; 2, auxilliary fire retardant and main flame retardant can not act synergistically, and flame retarding efficiency is low, and the impact resistance of product is poor, and transparency reduces; 3, must use light diffusing agent, it is white vaporific that the product that makes is, and transmittance is low, is merely 66-85%, can not satisfy the requirement of outdoor lighting Gao Guang; 4, the product light transmission and the flame retardant resistance that make are relatively poor.
Summary of the invention
The high transmission rate, the high flame retardant polycarbonate material that the objective of the invention is to be directed against the deficiency of prior art and a kind of light transmission and good flame resistance are provided.
Another object of the present invention is to a kind of high transmission rate, high flame retardant to be provided, satisfy the preparation method of the polycarbonate material that the high light of outdoor lighting requires to the deficiency of prior art.
The object of the invention is realized through following technical measures.
A kind of high transmission rate, high flame retardant polycarbonate material are provided, comprise the raw material of following component and mass percent:
Polycarbonate 94.8-99.5%
Fire retardant A 0.1-0.3%
Fire retardant B 0.1-3.5%
Inhibitor A 0.1-0.3%
Inhibitor B 0.1-0.3%
Lubricant 0.1-0.2%
Photostabilizer 0-0.6%
Wherein, said fire retardant A is a sulfobenzide sulphonate; Said fire retardant B is the bromination carbonate oligomer;
Wherein, said inhibitor A is tricresyl phosphite (2, a 4-di-tert-butyl) ester; Said inhibitor B is β-positive octadecanol ester of (3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid;
Wherein, said lubricant is octadecanoic acid-2-(methylol)-2-[[(1-oxo octadecyl) oxygen base] methyl]-1,3-glyceryl ester;
Wherein, said photostabilizer is a UV-531;
Wherein, the mass percent sum of above each component is 100%.
Wherein, said fire retardant A is a sulfobenzide sulphonate.
Sulfobenzide sulphonate (being commonly called as " KSS " or " KSS-FR "); Can use separately; Or with the organic silicon flame-retardant synergist and the usefulness of special construction, or with agent of high-molecular weight organophosphorus ester flame-proof and usefulness, make transparent or semitransparent halogen-free and flame-retardant polycarbonate (PC) material.Sulfobenzide sulphonate is reactive flame retardant, is used for the flame-retardant modified of polycarbonate material, can keep the original transparency of polycarbonate material; Addition is merely 0.1%-0.3%, can reach the fire-retardant requirement of UL 94 V-0 levels.KSS-FR is very little to the influence of the optical transparence of polycarbonate and other physical and mechanical properties.Sulfobenzide sulphonate has advantages such as good dispersivity, flame retarding efficiency height, clear polycarbonate good combination property.
Wherein, said fire retardant B is the bromination carbonate oligomer.
(Brominated Carbonated Oligomer BCO) is a kind of of Polymerized Brominated Flame Retardant to the brominated polycarbonate oligopolymer.The principal feature of Polymerized Brominated Flame Retardant: 1, Polymerized Brominated Flame Retardant is the polymer additive, has good consistency with superpolymer, does not separate out.2, has excellent photo and thermal stability.As Albemarle gather SAYTEX HP-3010, HP-7010 N2 protection, 320 ℃ down experience 60min rate of weight loss be merely 5%.HP-3010 is heated to 340 ℃ under the N2 protection, molecular weight still keeps 80%.3, can not generate many halogenated diphenyls and dioxan and many halogenated diphenyls and mutter.4, nontoxicity comprises its terminal applies product, no any rules of forbidding in the world wide.5, good fluidity, Technological adaptability is good.As the MFR of HP-3010 reached 67g/10min (235 ℃, 2.16kg).6, the moulding to thin-walled and the part with complicated structure is easier, helps shortening shaping cycle, enhances productivity.7, can reclaim and repeatability is used.8, can reach the strictest flame-retardant standard UL94, V-0 level.
In addition, bromination carbonate oligomer and above-mentioned sulfobenzide sulphonate synergistic are as fire retardant, and as the fire retardant use of transparent polycarbonate material, flame retardant properties is good.
Wherein, said inhibitor A is tricresyl phosphite (2, a 4-di-tert-butyl) ester.
Be commonly called as: oxidation inhibitor 168; Molecular mass: 646.93166; Fusing point: 181-184 ℃ white crystalline powder, is dissolved in benzene, toluene, gasoline, water insoluble and alcohols by fusing point 180-186 ℃.These article are low volatility organic synthesis antioxygen stopper; Be widely used in Vestolen PP 7052, Vilaterm, ABS, gather the synthetic of all types of plastic such as carbonic acid fiber and vibrin and process; Effectively prevent the thermal-oxidative degradation of material in extruding mixing process; Effectively improve product transparency, resistance to impact shock and transparence, prevent the product yellow.
Wherein, said inhibitor B is β-positive octadecanol ester of (3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid.
β-positive octadecanol the ester of (3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid is commonly called as: antioxidant 1076; , molecular weight: 530.88; Fusing point: 50-52 ℃; White crystalline powder.Fusing point 50-55 ℃, be dissolved in benzene, acetone, ester class, water insoluble.Be a kind of good oxidation inhibitor; Better heat-resisting and water-fast extraction ability are arranged; Be widely used in polyolefine, polyoxymethylene, ABS resin and various rubber and petroleum products; Effectively prevent the thermal-oxidative degradation of material in extruding mixing process, effectively improve product transparency, resistance to impact shock and transparence, prevent the product yellow.
Wherein, said lubricant is octadecanoic acid-2-(methylol)-2-[[(1-oxo octadecyl) oxygen base] methyl]-1,3-glyceryl ester.
Molecular formula is C59H114O7, molecular weight: 935.53226, and boiling point: 859.3 ° of Cat760mmHg, specific refractory power: 1.47, shining point: 213.6 ° of C, density: 0.925g/cm3, the processing plasticizing that helps the material extrusion is lubricated.Its interior lubricated and outer lubricated effect of lubricant, wherein, interior lubricating is meant that lubricant helps material and is uniformly dispersed, and makes things convenient for the subsequent product moulding and the demoulding, the wherein outer lubricated lubricant that is meant is convenient to the material demoulding and extrusion moulding, improves Drawing abillity.
Certainly, lubricant of the present invention can also be that the trade mark that Indonesia CMS produces is that the trade mark of the great power Chemical Manufacture in EBS lubricant, Zhengzhou of B-50 is that Magnesium Stearate (MGST) lubricant or the husky trade mark of producing of dragon of SM100 is the 120P lubricant of PETS.
The trade mark that Indonesia CMS produces is that the EBS lubricant of B-50 is an ethylene bis stearamide; Molecular formula is C18H76N2O2, is white to pale yellow powder or saccharoid, and fusing point is 130-145 ℃; Specific density is 0.98 (25 ℃); Flash-point is about 285 ℃, and it is water insoluble to be insoluble to most of usual vehicles such as ethanol, acetone, tetracol phenixin under the normal temperature, but meal has wetting properties more than 80 ℃.As lubricant, do not influence thermostability, appearance, the tone of plastics, transparency of film etc.
The trade mark of the great power Chemical Manufacture in Zhengzhou is that Magnesium Stearate (MGST) lubricant of SM100 is a Magnesium Stearate, and molecular formula is (C17H35COO) 2Mg, another name: magnesium octadecanate, SM100.Magnesium Stearate is white or milky uniform powder, and is tasteless, density 1.07, fusing point 108-115 ℃.Be slightly soluble in water, be slightly soluble in hot alcohol and benzene, dissolve in hot ethanol.Meet strong acid and can resolve into Triple Pressed Stearic Acid and corresponding magnesium salts, water absorbability is arranged, nontoxic, the particle of processing has good flowability and compressibility.
The 120P lubricant that the husky trade mark of producing of dragon is PETS is that structure is the high temperature lubricant of pentaerythritol stearate, and outward appearance is white powder, fusing point 60-65 Max; Acid number 2 Max; Hydroxyl value 12 Max, saponification value 195Max, the thermogravimetric analysis result shows; In the time of 350 ℃, PETS does not still have tangible weight loss; In the time of 375 ℃, weight loss about 2.5%; During to 400 ℃, it just begins to decompose (weight loss about 7%).PETS at high temperature has good thermostability and low volatility; The good demoulding and flowing property; Plastics to partial crystallization have fabulous nucleogenesis.Extrude with the mold course of processing in, PETS is an effective lubricating agent concerning a lot of polymkeric substance; Recommendation is used for the outstanding thermostability of PC (polycarbonate), thermoplastic polyester (PET, PBT etc.), PPO, PPS and other thermoplastic engineering plastic .PETS, makes it can be used for the course of processing of this type of system, does not worry degrading; And it can significantly improve transparency and surface smoothness.During as the external lubricant of PC, hard PVC and other polymeric system, the high efficiency of PETS allows its usage quantity to be lower than most of traditional lubricants, typical amounts 0.1～1%.In the time need possessing the demolding performace of thermostability and excellence simultaneously, PETS is a fabulous selection.
Wherein, said photostabilizer is a UV-531.
Molecular weight: 326.43, fusing point: 47-49 ℃, light yellow crystal is soluble in benzene, normal hexane, acetone, is dissolved in ethanol slightly, is slightly soluble in ethylene dichloride.Be the remarkable efficient anti-aging auxiliary agent of a kind of performance, can absorb the 300-375nm UV-light, have that look shallow is, nontoxic, consistency is good, transport property is little, be easy to characteristics such as processing.It has maximum provide protection to polymkeric substance, and helps to reduce color and luster, delays the rational loss of energy of yellowing and blocker simultaneously.Be widely used in aspects such as PE, PVC, PP, PS, PC, synthetic glass, polypropylene fiber and ethene acetic acid,, give material light aging resisting and xanthochromia performance for they provide good light stabilising effect.
Preferably, a kind of high transmission rate, high flame retardant polycarbonate material comprise the raw material of following component and mass percent:
Polycarbonate 95.8-97.4%
Fire retardant A 0.1-0.3%
Fire retardant B 1.5-3.0%
Inhibitor A 0.1-0.3%
Inhibitor B 0.1-0.3%
Lubricant 0.1-0.2%
Photostabilizer 0.1-0.6%.
More preferably, a kind of high transmission rate, high flame retardant polycarbonate material comprise the raw material of following component and mass percent:
Polycarbonate 96.5-97.4%
Fire retardant A 0.1-0.3%
Fire retardant B 1.5-3.0%
Inhibitor A 0.1-0.2%
Inhibitor B 0.1-0.2%
Lubricant 0.1-0.2%
Photostabilizer 0.3-0.6%.
Wherein, said polycarbonate is a bisphenol A polycarbonate, and molecular weight is 26000-40000.
Bisphenol A polycarbonate, formal name used at school are 2,2-pair (4 '-hydroxy phenyl) the propane polycarbonate.Molecular backbone chain contains the polycarbonate of dihydroxyphenyl propane ester structure.Tasteless, odorless, nontoxic transparent amorphous solid.Stable to diluted acid, oxygenant, reductive agent, aliphatic hydrocarbon etc., not alkaline-resisting, amine, ketone, fat and aromatic hydrocarbon are soluble in hydrochloric ether.Have over-all propertieies such as good heat, electricity and machinery, particularly shock-resistant, good toughness, creep are little, and product size is stable.Can be at-60～110 ℃ of life-time service, 135 ℃ of heat-drawn wires (1.82MPa), 149 ℃ of second-order transition temperatures, no sharp melting point, heat decomposition temperature>310 ℃; Water-absorbent is little, and electrical properties in high temperatures is good.The branch of light phosgenation polycarbonate and ester-interchange method polycarbonate is arranged, and performance is slightly variant.Bisphenol A polycarbonate adopts the middle HMW of 26000-40000, and forming stability is good, helps injection moulding and extrusion moulding in the product processing, and product light transmission, impact resistance, resistance toheat are good, and notched Izod impact strength is high.
The bisphenol A polycarbonate that the present invention selects for use be Bayer AG 2805, the 1250Z of Supreme Being people company or the 1201-10 of the Dow Chemical Company.The molecular weight of the bisphenol A polycarbonate of these three kinds of specifications all is about about 30000, and the flowability of product is bigger, and flowing property is about 10, help the following process moulding, and raw material sources is extensive.
Wherein, the ratio of the mass percent of said fire retardant A and said fire retardant B is 1:1.
Wherein, the ratio of the mass percent of said inhibitor A and said inhibitor B is 1:1.The weight ratio of oxidation inhibitor A of the present invention and oxidation inhibitor B is preferably 1:1, helps improving the transmittance of product.
Another object of the present invention realizes through following technical scheme.
The preparation method of a kind of high transmission rate, high flame retardant polycarbonate material is provided, comprises following process step:
The first step: fire retardant A, fire retardant B, oxidation inhibitor A, fire retardant B, lubricant, photostabilizer are put into impeller and stirred, and stirring velocity is 100-200r/min, and churning time is 2-4min; The thorough mixing that helps material is even, helps the following process moulding.
Second step: the material of polycarbonate and the first step mixing is put into impeller together carry out syllogic and stir; The stirring velocity of first section stirring is 20-50r/min; Churning time is 1-4min, and the stirring velocity of second section stirring is 100-200r/min, and churning time is 1-4min; The stirring velocity of the 3rd section stirring is 10-50r/min, and churning time is 1-4min; Adopt slow, fast, slow syllogic to stir, it is even to help the material thorough mixing, avoids particle and material layering, and can avoid occurring stirring the dead angle, and mixing effect is good, helps improving the quality of products.
The 3rd step: second step was mixed material put into twin screw extruder and carry out extruding pelletization; Pellet feeding section extrusion temperature is: 230-250 ℃, the fluxing zone extrusion temperature is: 250-270 ℃, the melt conveying zone extrusion temperature is: 250-270 ℃, head temperature is: 240-260 ℃, the vacuum tightness that extruding pelletization adds man-hour is 0.6MPa-0.8MPa.To the strict control of the temperature of each course of processing in the product prepn process, guarantee the full and uniform fusion of material, the product light transmission is good, and flame retardant properties is high.
Preferably, in the said the first step, stirring velocity is 120-180r/min, and churning time is 2-3min.
Preferably, in said second step, the churning time of first section stirring is 2min, and the churning time of second section stirring is 2min, and the churning time of the 3rd section stirring is 1min.
Preferably, in said the 3rd step, pellet feeding section extrusion temperature is: 235-245 ℃; The fluxing zone extrusion temperature is: 255-265 ℃; The melt conveying zone extrusion temperature is: 255-265 ℃, head temperature is: 245-255 ℃, the vacuum tightness that extruding pelletization adds man-hour is 0.65MPa-0.75MPa.
Beneficial effect of the present invention is: a kind of high transmission rate of the present invention, high flame retardant polycarbonate material; The raw material that comprises following component and mass percent: polycarbonate 94.8-99.5%, fire retardant A0.1-0.3%, fire retardant B0.1-3.5%, inhibitor A0.1-0.3%, inhibitor B0.1-0.3%, lubricant 0.1-0.2%, photostabilizer 0-0.6%; Wherein, the mass percent sum of above each component is 100%.Its preparation method comprises following process step: the first step: fire retardant A, fire retardant B, oxidation inhibitor A, fire retardant B, lubricant, photostabilizer are put into impeller and stirred, and stirring velocity is 100-200r/min, and churning time is 2-4min; Second step: the material of polycarbonate and the first step mixing is put into impeller together carry out syllogic and stir; The stirring velocity of first section stirring is 20-50r/min; Churning time is 1-4min, and the stirring velocity of second section stirring is 100-200r/min, and churning time is 1-4min; The stirring velocity of the 3rd section stirring is 10-50r/min, and churning time is 1-4min; The 3rd step: second step was mixed material put into twin screw extruder and carry out extruding pelletization; Pellet feeding section extrusion temperature is: 230-250 ℃, the fluxing zone extrusion temperature is: 250-270 ℃, the melt conveying zone extrusion temperature is: 250-270 ℃, head temperature is: 240-260 ℃, the vacuum tightness that extruding pelletization adds man-hour is 0.6MPa-0.8MPa.The polycarbonate material that the present invention makes has the advantage of light transmission and good flame resistance, can satisfy the requirement of outdoor lighting with lampshade, and technology is simple, ripe, and production cost is low, helps generally applying.
Advantage of the present invention has: (1) is keeping having kept the high transmission rate of material more than 90% under polycarbonate high flame retardant effect (2.0mm V0) prerequisite.
(2) consumption of main flame retardant is less, and the shock resistance of the polycarbonate material that makes is up to 600-700, and the IZOD notched Izod impact strength is high, and not easily broken during the product assembling, structural strength is high, and is practical.
(3) auxilliary fire retardant can act synergistically with main flame retardant, and flame retarding efficiency is high, and the impact resistance of product is good, and transparency is high.
(4) the product melting index that makes is constant, and the thermal stability of product is good between 10-11 (ASTM D1238), and mold temperature is moderate, effectively avoids product surface scalelike mark to occur, and quality product is high.
The flame retardant resistance of the product that (5) makes is 2.0mm (V2, V0), and flame retardant properties is high, and matches with the thickness (2.0mm) of the light fixture outer cover of existing standard outdoor illumination requirement just, helps generally applying.
The fluorescence burn-in test performance of the product that (6) makes is good, at irradiation intensity 0.55W/M 2Under the irradiation time 300H condition, reach △ E-3.5 to △ E-0.8, product is difficult for yellow, and product appearance is transparence, and stable performance, and lighting effect is good.
(7) polycarbonate material of the present invention also can reach high flame resistance when reaching the high light transmittance ability, and quality product is high, is fit to be applied to outdoor lighting and uses outer cover material, the product excellent combination property.
Embodiment
Below in conjunction with embodiment the present invention is further described, this is preferred embodiment of the present invention.
embodiment one.
A kind of high transmission rate of present embodiment, high flame retardant polycarbonate material; The raw material that comprises following component and mass percent: 2805 bisphenol A polycarbonate of 99.5% Bayer AG, 0.1% sulfobenzide sulphonate, 0.1% bromination carbonate oligomer, 0.1% tricresyl phosphite (2; The 4-di-tert-butyl) ester, 0.1% β-(3; The 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid, octadecanoic acid-2-(methylol)-2-[[(1-oxo octadecyl) oxygen base] methyl]-1 of 0.1%, 3-glyceryl ester.
Its preparation method is: the first step: the above-mentioned mass percent proportion raw material beyond the bisphenol A polycarbonate is put into impeller stir, stirring velocity is 100r/min, and churning time is 4min; Second step: the material of bisphenol A polycarbonate and the first step mixing is put into impeller together carry out syllogic and stir; The stirring velocity of first section stirring is 20r/min; Churning time is 4min, and the stirring velocity of second section stirring is 100r/min, and churning time is 4min; The stirring velocity of the 3rd section stirring is 10r/min, and churning time is 4min; The 3rd step: second step was mixed material put into twin screw extruder and carry out extruding pelletization; Pellet feeding section extrusion temperature is: 230 ℃, the fluxing zone extrusion temperature is: 250 ℃, the melt conveying zone extrusion temperature is: 250 ℃, head temperature is: 240 ℃, the vacuum tightness that extruding pelletization adds man-hour is 0.6MPa.
The polycarbonate material that the present invention makes, it is good to have a melting behaviour, and tensile strength is high; Elongation at break is greater than 80%, and flexural strength is high, and crooked elastic rate is high; The IZOD notched Izod impact strength is big, and heat-drawn wire is moderate, and full light is crossed the light rate and reached more than 90%; Fluorescence burn-in test performance is good, and the product appearance transparency is high, the advantage that flame retardant properties is good.
embodiment two.
A kind of high transmission rate of present embodiment, high flame retardant polycarbonate material; The raw material that comprises following component and mass percent: the bisphenol A polycarbonate of the 1250Z of 99.1% Supreme Being people company, 0.1% sulfobenzide sulphonate, 0.3% bromination carbonate oligomer, 0.1% tricresyl phosphite (2; The 4-di-tert-butyl) ester, 0.1% β-(3; The 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid, octadecanoic acid-2-(methylol)-2-[[(1-oxo octadecyl) oxygen base] methyl]-1 of 0.2%, 3-glyceryl ester and 0.1% UV-531.
Its preparation method is: the first step: the above-mentioned mass percent proportion raw material beyond the bisphenol A polycarbonate is put into impeller stir, stirring velocity is 140r/min, and churning time is 3min; Second step: the material of bisphenol A polycarbonate and the first step mixing is put into impeller together carry out syllogic and stir; The stirring velocity of first section stirring is 30r/min; Churning time is 3min, and the stirring velocity of second section stirring is 140r/min, and churning time is 3min; The stirring velocity of the 3rd section stirring is 20r/min, and churning time is 3min; The 3rd step: second step was mixed material put into twin screw extruder and carry out extruding pelletization; Pellet feeding section extrusion temperature is: 240 ℃, the fluxing zone extrusion temperature is: 260 ℃, the melt conveying zone extrusion temperature is: 260 ℃, head temperature is: 250 ℃, the vacuum tightness that extruding pelletization adds man-hour is 0.7MPa.
embodiment three.
A kind of high transmission rate of present embodiment, high flame retardant polycarbonate material; The raw material that comprises following component and mass percent: the bisphenol A polycarbonate of the 1201-10 of 98.6% the Dow Chemical Company, 0.2% sulfobenzide sulphonate, 0.7% bromination carbonate oligomer, 0.1% tricresyl phosphite (2; The 4-di-tert-butyl) ester, 0.1% β-(3; The 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid, octadecanoic acid-2-(methylol)-2-[[(1-oxo octadecyl) oxygen base] methyl]-1 of 0.2%, 3-glyceryl ester and 0.1% UV-531.
Its preparation method is: the first step: the above-mentioned mass percent proportion raw material beyond the bisphenol A polycarbonate is put into impeller stir, stirring velocity is 180r/min, and churning time is 3.5min; Second step: the material of bisphenol A polycarbonate and the first step mixing is put into impeller together carry out syllogic and stir; The stirring velocity of first section stirring is 40r/min; Churning time is 2min, and the stirring velocity of second section stirring is 180r/min, and churning time is 2min; The stirring velocity of the 3rd section stirring is 30r/min, and churning time is 2min; The 3rd step: second step was mixed material put into twin screw extruder and carry out extruding pelletization; Pellet feeding section extrusion temperature is: 245 ℃, the fluxing zone extrusion temperature is: 265 ℃, the melt conveying zone extrusion temperature is: 265 ℃, head temperature is: 255 ℃, the vacuum tightness that extruding pelletization adds man-hour is 0.75MPa.
embodiment four.
A kind of high transmission rate of present embodiment, high flame retardant polycarbonate material; The raw material that comprises following component and mass percent: 2805 bisphenol A polycarbonate of 98.1% Bayer AG, 0.2% sulfobenzide sulphonate, 1.0% bromination carbonate oligomer, 0.1% tricresyl phosphite (2; The 4-di-tert-butyl) ester, 0.1% β-(3; The 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid, octadecanoic acid-2-(methylol)-2-[[(1-oxo octadecyl) oxygen base] methyl]-1 of 0.2%, 3-glyceryl ester and 0.3% UV-531.
Its preparation method is: the first step: the above-mentioned mass percent proportion raw material beyond the bisphenol A polycarbonate is put into impeller stir, stirring velocity is 200r/min, and churning time is 2min; Second step: the material of bisphenol A polycarbonate and the first step mixing is put into impeller together carry out syllogic and stir; The stirring velocity of first section stirring is 50r/min; Churning time is 1min, and the stirring velocity of second section stirring is 200r/min, and churning time is 1min; The stirring velocity of the 3rd section stirring is 40r/min, and churning time is 1min; The 3rd step: second step was mixed material put into twin screw extruder and carry out extruding pelletization; Pellet feeding section extrusion temperature is: 250 ℃, the fluxing zone extrusion temperature is: 270 ℃, the melt conveying zone extrusion temperature is: 270 ℃, head temperature is: 260 ℃, the vacuum tightness that extruding pelletization adds man-hour is 0.8MPa.
embodiment five.
A kind of high transmission rate of present embodiment, high flame retardant polycarbonate material; The raw material that comprises following component and mass percent: the bisphenol A polycarbonate of the 1250Z of 97.6% Supreme Being people company, 0.2% sulfobenzide sulphonate, 1.4% bromination carbonate oligomer, 0.1% tricresyl phosphite (2; The 4-di-tert-butyl) ester, 0.1% β-(3; The 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid, octadecanoic acid-2-(methylol)-2-[[(1-oxo octadecyl) oxygen base] methyl]-1 of 0.2%, 3-glyceryl ester and 0.4% UV-531.
Its preparation method is: the first step: the above-mentioned mass percent proportion raw material beyond the bisphenol A polycarbonate is put into impeller stir, stirring velocity is 200r/min, and churning time is 2min; Second step: the material of bisphenol A polycarbonate and the first step mixing is put into impeller together carry out syllogic and stir; The stirring velocity of first section stirring is 50r/min; Churning time is 1min, and the stirring velocity of second section stirring is 200r/min, and churning time is 1min; The stirring velocity of the 3rd section stirring is 50r/min, and churning time is 1min; The 3rd step: second step was mixed material put into twin screw extruder and carry out extruding pelletization; Pellet feeding section extrusion temperature is: 250 ℃, the fluxing zone extrusion temperature is: 270 ℃, the melt conveying zone extrusion temperature is: 270 ℃, head temperature is: 260 ℃, the vacuum tightness that extruding pelletization adds man-hour is 0.8MPa.
embodiment six.
A kind of high transmission rate of present embodiment, high flame retardant polycarbonate material; The raw material that comprises following component and mass percent: 2805 bisphenol A polycarbonate of 97.1% Bayer AG, 0.1% sulfobenzide sulphonate, 2.0% bromination carbonate oligomer, 0.1% tricresyl phosphite (2; The 4-di-tert-butyl) ester, 0.1% β-(3; The 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid, octadecanoic acid-2-(methylol)-2-[[(1-oxo octadecyl) oxygen base] methyl]-1 of 0.1%, 3-glyceryl ester and 0.5% UV-531.
The preparation method of present embodiment is identical with embodiment one with the performance of products of preparing, and repeats no more here.
embodiment seven.
A kind of high transmission rate of present embodiment, high flame retardant polycarbonate material; The raw material that comprises following component and mass percent: the bisphenol A polycarbonate of the 1250Z of 95.6% Supreme Being people company, 0.3% sulfobenzide sulphonate, 3.0% bromination carbonate oligomer, 0.2% tricresyl phosphite (2; The 4-di-tert-butyl) ester, 0.2% β-(3; The 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid, octadecanoic acid-2-(methylol)-2-[[(1-oxo octadecyl) oxygen base] methyl]-1 of 0.1%, 3-glyceryl ester and 0.6% UV-531.
The preparation method of present embodiment is identical with embodiment two with the performance of products of preparing, and repeats no more here.
embodiment eight.
A kind of high transmission rate of present embodiment, high flame retardant polycarbonate material; The raw material that comprises following component and mass percent: the bisphenol A polycarbonate of the 1201-10 of 94.8% the Dow Chemical Company, 0.3% sulfobenzide sulphonate, 3.5% bromination carbonate oligomer, 0.3% tricresyl phosphite (2; The 4-di-tert-butyl) ester, 0.3% β-(3; The 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid, octadecanoic acid-2-(methylol)-2-[[(1-oxo octadecyl) oxygen base] methyl]-1 of 0.2%, 3-glyceryl ester and 0.6% UV-531.
The preparation method of present embodiment is identical with embodiment three with the performance of products of preparing, and repeats no more here.
Below be the each component of the foregoing description one to embodiment eight and the tabulation of mass percent thereof:
Sequence number Polycarbonate Fire retardant A Fire retardant B Inhibitor A Inhibitor B Lubricant Photostabilizer
Embodiment 1 99.5 0.1 0.1 0.1 0.1 0.1 0
Embodiment 2 99.1 0.1 0.3 0.1 0.1 0.2 0.1
Embodiment 3 98.6 0.2 0.7 0.1 0.1 0.2 0.1
Embodiment 4 98.1 0.2 1.0 0.1 0.1 0.2 0.3
Embodiment 5 97.6 0.2 1.4 0.1 0.1 0.2 0.4
Embodiment 6 97.1 0.1 2.0 0.1 0.1 0.1 0.5
Embodiment 7 95.6 0.3 3.0 0.2 0.2 0.1 0.6
Embodiment 8 94.8 0.3 3.5 0.3 0.3 0.2 0.6
Below be each item performance testing index of the polycarbonate material processed of the component raw material of the foregoing description one to embodiment eight:
Figure 833889DEST_PATH_IMAGE002
Can find out from each item performance testing index of above-mentioned polycarbonate material; The polycarbonate material that the present invention makes has high printing opacity, high flame resistance, and product appearance is transparent, and it is high that full light is crossed the light rate; Satisfy the requirement of outdoor lighting high brightness, be suitable for making outdoor lighting and use lampshade; The stable performance of fluorescence burn-in test, product is difficult for aging and yellow, and quality product is high, long service life; The fracture extensibility is big, the IZOD notched Izod impact strength is high, and installation process is not fragile, and is practical.
Should be noted that at last; Above embodiment is only in order to explain technical scheme of the present invention; But not to the restriction of protection domain of the present invention, although with reference to preferred embodiment the present invention has been done explanation at length, those of ordinary skill in the art is to be understood that; Can make amendment or be equal to replacement technical scheme of the present invention, and not break away from the essence and the scope of technical scheme of the present invention.

Claims (10)

1. a high transmission rate, high flame retardant polycarbonate material is characterized in that: the raw material that comprises following component and mass percent:
Polycarbonate 94.8-99.5%
Fire retardant A 0.1-0.3%
Fire retardant B 0.1-3.5%
Inhibitor A 0.1-0.3%
Inhibitor B 0.1-0.3%
Lubricant 0.1-0.2%
Photostabilizer 0-0.6%
Wherein, said fire retardant A is a sulfobenzide sulphonate; Said fire retardant B is the bromination carbonate oligomer;
Wherein, said inhibitor A is tricresyl phosphite (2, a 4-di-tert-butyl) ester; Said inhibitor B is β-positive octadecanol ester of (3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid;
Wherein, said lubricant is octadecanoic acid-2-(methylol)-2-[[(1-oxo octadecyl) oxygen base] methyl]-1,3-glyceryl ester;
Wherein, said photostabilizer is a UV-531;
Wherein, the mass percent sum of above each component is 100%.
2. a kind of high transmission rate according to claim 1, high flame retardant polycarbonate material is characterized in that: the raw material that comprises following component and mass percent:
Polycarbonate 95.8-97.4%
Fire retardant A 0.1-0.3%
Fire retardant B 1.5-3.0%
Inhibitor A 0.1-0.3%
Inhibitor B 0.1-0.3%
Lubricant 0.1-0.2%
Photostabilizer 0.1-0.6%.
3. a kind of high transmission rate according to claim 1, high flame retardant polycarbonate material is characterized in that: the raw material that comprises following component and mass percent:
Polycarbonate 96.5-97.4%
Fire retardant A 0.1-0.3%
Fire retardant B 1.5-3.0%
Inhibitor A 0.1-0.2%
Inhibitor B 0.1-0.2%
Lubricant 0.1-0.2%
Photostabilizer 0.3-0.6%.
4. a kind of high transmission rate according to claim 1, high flame retardant polycarbonate material is characterized in that: said polycarbonate is a bisphenol A polycarbonate, and molecular weight is 26000-40000.
5. a kind of high transmission rate according to claim 1, high flame retardant polycarbonate material is characterized in that: said bisphenol A polycarbonate be Bayer AG 2805, the 1250Z of Supreme Being people company or the 1201-10 of the Dow Chemical Company.
6. a kind of high transmission rate according to claim 1, high flame retardant polycarbonate material is characterized in that: the ratio of the mass percent of said inhibitor A and said inhibitor B is 1:1.
7. the preparation method of any described a kind of high transmission rate, high flame retardant polycarbonate material among the claim 1-6 is characterized in that: comprise following process step:
The first step: fire retardant A, fire retardant B, oxidation inhibitor A, fire retardant B, lubricant, photostabilizer are put in the impeller successively and stirred, and stirring velocity is 100-200r/min, and churning time is 2-4min;
Second step: the material of polycarbonate and the first step mixing is put into impeller together carry out syllogic and stir; The stirring velocity of first section stirring is 20-50r/min; Churning time is 1-4min, and the stirring velocity of second section stirring is 100-200r/min, and churning time is 1-4min; The stirring velocity of the 3rd section stirring is 10-50r/min, and churning time is 1-4min;
The 3rd step: second step was mixed material put into twin screw extruder and carry out extruding pelletization; Pellet feeding section extrusion temperature is: 230-250 ℃, the fluxing zone extrusion temperature is: 250-270 ℃, the melt conveying zone extrusion temperature is: 250-270 ℃, head temperature is: 240-260 ℃, the vacuum tightness that extruding pelletization adds man-hour is 0.6MPa-0.8MPa.
8. the preparation method of a kind of high transmission rate according to claim 7, high flame retardant polycarbonate material is characterized in that: in the said the first step, stirring velocity is 120-180r/min, and churning time is 2-3min.
9. the preparation method of a kind of high transmission rate according to claim 7, high flame retardant polycarbonate material; It is characterized in that: in said second step; The churning time of first section stirring is 2min, and the churning time of second section stirring is 2min, and the churning time of the 3rd section stirring is 1min.
10. the preparation method of a kind of high transmission rate according to claim 7, high flame retardant polycarbonate material; It is characterized in that: in said the 3rd step; Pellet feeding section extrusion temperature is: 235-245 ℃, the fluxing zone extrusion temperature is: 255-265 ℃, the melt conveying zone extrusion temperature is: 255-265 ℃; Head temperature is: 245-255 ℃, the vacuum tightness that extruding pelletization adds man-hour is 0.65MPa-0.75MPa.
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CN106280379A (en) * 2016-09-30 2017-01-04 福建华塑新材料有限公司 A kind of high transmission rate Merlon and preparation method thereof
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CN103044890A (en) * 2012-12-31 2013-04-17 广东银禧科技股份有限公司 Lusterless polycarbonate material and preparation method thereof
CN103044890B (en) * 2012-12-31 2016-04-20 广东银禧科技股份有限公司 A kind of dumb light polycarbonate material and preparation method thereof
CN103044893A (en) * 2013-01-28 2013-04-17 浙江赛日新材料科技有限公司 Polycarbonate with high light transmittance
CN103044893B (en) * 2013-01-28 2015-07-08 浙江赛日新材料科技有限公司 Polycarbonate with high light transmittance
CN103822118A (en) * 2014-01-28 2014-05-28 徐松炎 Light-transmitting LED (light-emitting diode) waterproof lamp group and manufacturing method thereof
CN105542424A (en) * 2016-01-26 2016-05-04 湖北工程学院 Flame-retardant, high-transmittance and weather-proof polycarbonate composite used for LED lampshade and preparation method
CN106280379A (en) * 2016-09-30 2017-01-04 福建华塑新材料有限公司 A kind of high transmission rate Merlon and preparation method thereof
CN106280378A (en) * 2016-09-30 2017-01-04 福建华塑新材料有限公司 One is exempted to spray polycarbonate compositions and preparation method thereof
CN106398162A (en) * 2016-09-30 2017-02-15 福建华塑新材料有限公司 Polycarbonate for warm-light LED lampshade and preparation method thereof
CN106433071A (en) * 2016-09-30 2017-02-22 福建华塑新材料有限公司 Halogen-free flame-retardant polycarbonate composition and preparation method thereof
CN106433072A (en) * 2016-09-30 2017-02-22 福建华塑新材料有限公司 High thermal conductivity polycarbonate resin composition and preparation method thereof
CN109111712A (en) * 2018-07-17 2019-01-01 广东聚石化学股份有限公司 A kind of low smell fire retardation PC material and preparation method thereof

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