CN102702716B - 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
CN102702716B
CN102702716B CN201210221193.4A CN201210221193A CN102702716B CN 102702716 B CN102702716 B CN 102702716B CN 201210221193 A CN201210221193 A CN 201210221193A CN 102702716 B CN102702716 B CN 102702716B
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polycarbonate
antioxidant
fire retardant
churning time
flame retardant
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CN102702716A (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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GUANGDONG SILVERAGE HOLDINGS 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

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

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 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) because its volume is little, the life-span long, the plurality of advantages such as abundant and outstanding energy-conserving and environment-protective characteristic that develop the color obtain increasingly extensive application in fields such as demonstration, traffic, electrical equipment and illuminations, be one of gordian technique of China's energy-saving and emission-reduction, cleaner production and Sustainable development.
LED is due to the characteristics of luminescence of its pointolite, is being applied to the weak point that has on lighting field that lighting area is little, brightness of illumination is low etc. with respect to conventional light source.The deficiency of applying on lighting field for making up LED light source, need to change the characteristics of luminescence of its pointolite into area source by exotic materials, keeps higher transmittance simultaneously.
Polycarbonate material because its intensity is high, transparent, high thermal resistance and flame retardant resistance, conventionally selected is lighting outer cover material.When the polycarbonate of non-modified is used as light fixture outer cover; flame retardant properties is lower; need to carry out special flame-retardant modified with protection LED lamp source, prevent that lamp source is destroyed or be subject to sun exposure and variable color; but when as LED outdoor lighting lamp outer cover; polycarbonate outer cover can cause transmittance to decline through traditional after flame-retardant modified; there is the problem that luminous efficiency is low, cannot bring into play the feature of LED illumination high brightness.
Chinese Patent Application No. is 2011110151541.0 patent of invention, announce a kind of LED light fixture flame-retarding light-diffusing polycarbonate resin composite and preparation method thereof, comprise the component of following mass percent composition: 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%.But there is following shortcoming in this documents: 1, the large usage quantity of main flame retardant, the shock resistance of the polycarbonate material making is poor, only can reach the IZOD notched Izod impact strength of 100-200, easily cracked when assembling product, in addition, cause the easy flavescence of product later stage, quality product declines; 2, auxiliary 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 making is, and transmittance is low, is only 66-85%, can not meet the requirement of outdoor lighting Gao Guang; 4, the product light transmission and the flame retardant resistance that make are poor.
Summary of the invention
The object of the invention is to provide for the deficiencies in the prior art high transmission rate, the high flame retardant polycarbonate material of a kind of light transmission and good flame resistance.
Another object of the present invention is to the preparation method who provides a kind of high transmission rate, high flame retardant for the deficiencies in the prior art, meets the polycarbonate material of the high light requirement of outdoor lighting.
Object of the present invention realizes by 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%
Antioxidant A 0.1-0.3%
Antioxidant B 0.1-0.3%
Lubricant 0.1-0.2%
Photostabilizer 0-0.6%
Wherein, described fire retardant A is sulfobenzide sulfonate; Described fire retardant B is bromination carbonate oligomer;
Wherein, described antioxidant A is tricresyl phosphite (2,4-di-tert-butyl) ester; Described antioxidant B is the positive octadecanol ester of β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid;
Wherein, described lubricant is octadecanoic acid-2-(methylol)-2-[[(1-oxo octadecyl) oxygen base] methyl]-1,3-glyceryl ester;
Wherein, described photostabilizer is Octabenzone;
Wherein, the mass percent sum of above each component is 100%.
Wherein, described fire retardant A is sulfobenzide sulfonate.
Sulfobenzide sulfonate (being commonly called as " KSS " or " KSS-FR "), can be used alone, or with organic silicon flame-retardant synergist the use of special construction, or with organophosphorus ester flame-proof agent the use of high molecular, manufacture transparent or semitransparent halogen-free and flame-retardant polycarbonate (PC) material.Sulfobenzide sulfonate is reactive flame retardant, and flame-retardant modified for polycarbonate material can keep the original transparency of polycarbonate material; Addition is only 0.1%-0.3%, can reach the fire-retardant requirement of UL 94 V-0 levels.The impact of the optical transparence of KSS-FR on polycarbonate and other physical and mechanical properties is very micro-.Sulfobenzide sulfonate has the advantages such as good dispersity, flame retarding efficiency are high, clear polycarbonate good combination property.
Wherein, described fire retardant B is bromination carbonate oligomer.
Brominated polycarbonate oligopolymer (Brominated Carbonated Oligomer, BCO) is the one of Polymerized Brominated Flame Retardant.The principal feature of Polymerized Brominated Flame Retardant: 1, Polymerized Brominated Flame Retardant is polymer additive, has good consistency with superpolymer, does not separate out.2, there is excellent photo and thermal stability.Be only 5% as poly-SAYTEX HP-3010, the HP-7010 of Albemarle experience 60min rate of weight loss at N2 protection, 320 ℃.HP-3010, under N2 protection, is heated to 340 ℃, and molecular weight still retains 80%.3, can not generate many halogenated diphenyls dioxan and many halogenated diphenyls and mutter.4, nontoxicity, comprises its terminal applies product, and world wide is interior without any rules of forbidding.5, good fluidity, Technological adaptability is good.As the MFR of HP-3010 has reached 67g/10min(235 ℃, 2.16kg).6, easier to the moulding of thin-walled and the part with complicated structure, be conducive to shorten shaping cycle, enhance productivity.7, can reclaim and use repeatly.8, can reach the strictest flame-retardant standard UL94, V-0 level.
In addition, bromination carbonate oligomer and above-mentioned sulfobenzide sulfonate synergistic, as fire retardant, use as the fire retardant of transparent polycarbonate material, and flame retardant properties is good.
Wherein, described antioxidant A is tricresyl phosphite (2,4-di-tert-butyl) ester.
Be commonly called as: irgasfos 168; Molecular mass: 646.93166; Fusing point: 181-184 ℃ white crystalline powder, fusing point 180-186 ℃, is dissolved in benzene, toluene, gasoline, water insoluble and alcohols.These product are the agent of low volatility organic synthesis resistance to the oxygen inhibiting polymerization, be widely used in the synthetic and processing of all types of plastic such as polypropylene, polyethylene, ABS, poly-carbonic acid fiber and vibrin, effectively prevent that material is at the thermal-oxidative degradation of extruding in mixing process, effectively improve product transparency, resistance to impact shock and transparence, prevent product yellow.
Wherein, described antioxidant B is the positive octadecanol ester of β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid.
The positive octadecanol ester of β-(3,5-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 ℃, is dissolved in benzene, acetone, ester class, water insoluble.A kind of good oxidation inhibitor, there is heat-resisting and water-fast extraction ability preferably, be widely used in polyolefine, polyoxymethylene, ABS resin and various rubber and petroleum products, effectively prevent that material is at the thermal-oxidative degradation of extruding in mixing process, effectively improve product transparency, resistance to impact shock and transparence, prevent product yellow.
Wherein, described 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 is conducive to material extrusion is lubricated.Lubricant is lubricated and outer lubricated effect in it, and wherein, interior lubricated to refer to that lubricant is conducive to material dispersion even, facilitates subsequent product moulding and the demoulding, and its China and foreign countries are lubricated refers to that lubricant is convenient to the material demoulding and extrusion moulding, improves Drawing abillity.
Certainly, lubricant of the present invention can also be the 120P lubricant that the trade mark of the trade mark that Indonesia CMS the produces great power Chemical Manufacture in EBS lubricant, Zhengzhou that is B-50 Magnesium Stearate (MGST) lubricant that is SM100 or the husky trade mark of producing of dragon are PETS.
The EBS lubricant that the trade mark that Indonesia CMS produces is B-50 is ethylene bis stearamide, molecular formula is C18H76N2O2, for white is to pale yellow powder or saccharoid, fusing point is 130-145 ℃, relative density is 0.98(25 ℃), flash-point is 285 ℃ of left and right, be insoluble to most of usual vehicles such as ethanol, acetone, tetracol phenixin water insoluble, but meal has wetting properties above at 80 ℃ under normal temperature.As lubricant, do not affect thermostability, appearance, the tone of plastics, transparency of film etc.
Magnesium Stearate (MGST) lubricant that the trade mark of the great power Chemical Manufacture in Zhengzhou is SM100 is Magnesium Stearate, and molecular formula is (C17H35COO) 2Mg, another name: magnesium octadecanate, SM100.Magnesium Stearate is white or milky uniform powder, 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 stearic acid and corresponding magnesium salts, have water absorbability, nontoxic, the particle of making has good mobility 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, outward appearance is white powder, fusing point 60-65 Max, acid number 2 Max, hydroxyl value 12 Max, saponification value 195Max, thermogravimetric analysis result shows, 350 ℃ time, PETS does not still have obvious weight loss; 375 ℃ time, weight loss approximately 2.5%; During to 400 ℃, it just starts to decompose (weight loss approximately 7%).PETS at high temperature has good thermostability and low volatility; The good demoulding and flowing property; The plastics of partial crystallization are had to fabulous nucleogenesis.Extrude with the mold course of processing in, PETS is an effective lubricant concerning a lot of polymkeric substance; Recommend for PC (polycarbonate), thermoplastic polyester (PET, PBT etc.), PPO, PPS and other the outstanding thermostability of thermoplastic engineering plastic .PETS, make it can be used for the course of processing of this type of system, do 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 lower than most of traditional lubricants, typical amounts 0.1～1%.In the time need to possessing thermostability and excellent demolding performace, PETS is a fabulous selection simultaneously.
Wherein, described photostabilizer is Octabenzone.
Molecular weight: 326.43, fusing point: 47-49 ℃, light yellow crystal, is soluble in benzene, normal hexane, acetone, is slightly dissolved in ethanol, is slightly soluble in ethylene dichloride.Be a kind of efficient anti-aging auxiliary agent of performance brilliance, can absorb 300-375nm UV-light, have that look shallow is, nontoxic, consistency is good, transport property is little, be easy to the features such as processing.It has maximum provide protection to polymkeric substance, and contributes to reduce color and luster, delays yellowing and the blocker rationality loss of energy simultaneously.Be widely used in the aspects such as PE, PVC, PP, PS, PC, synthetic glass, polypropylene fiber and ethene acetic acid, for they provide good light stabilising effect, give material light aging resisting and xanthochromia performance.
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%
Antioxidant A 0.1-0.3%
Antioxidant 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%
Antioxidant A 0.1-0.2%
Antioxidant B 0.1-0.2%
Lubricant 0.1-0.2%
Photostabilizer 0.3-0.6%.
Wherein, described polycarbonate is bisphenol A polycarbonate, and molecular weight is 26000-40000.
Bisphenol A polycarbonate, formal name used at school is two (4 '-hydroxy phenyl) the propane polycarbonate of 2,2-.Molecular backbone chain is containing 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, be soluble in hydrochloric ether.Have good heat, electricity and the over-all properties such as mechanical, 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, without sharp melting point, heat decomposition temperature >310 ℃; Water-absorbent is little, and electrical properties in high temperatures is good.Have dividing of light phosgenation polycarbonate and ester-interchange method polycarbonate, performance is slightly variant.Bisphenol A polycarbonate adopts the middle high molecular of 26000-40000, and forming stability is good, is conducive to injection moulding and extrusion moulding in 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 be Bayer AG 2805, the 1250Z of Di Ren company or the 1201-10 of the Dow Chemical Company.The molecular weight of the bisphenol A polycarbonate of these three kinds of specifications is all about 30000 left and right, and the mobility of product is larger, and flowing property is about 10, be conducive to following process moulding, and raw material sources is extensive.
Wherein, the ratio of the mass percent of described fire retardant A and described fire retardant B is 1:1.
Wherein, the ratio of the mass percent of described antioxidant A and described antioxidant B is 1:1.The weight ratio of oxidation inhibitor A of the present invention and oxidation inhibitor B is preferably 1:1, is conducive to improve the transmittance of product.
Another object of the present invention, is achieved through the following technical solutions.
The preparation method that a kind of high transmission rate, high flame retardant polycarbonate material are provided, comprises following processing step:
The first step: fire retardant A, fire retardant B, oxidation inhibitor A, fire retardant B, lubricant, photostabilizer are put into homogenizer and stirred, and stirring velocity is 100-200r/min, and churning time is 2-4min; Be conducive to fully mixing of material, be conducive to following process moulding.
Second step: put into homogenizer together with the material that polycarbonate is mixed with the first step and carry out syllogic and stir evenly, the stirring velocity that first paragraph stirs is 20-50r/min, churning time is 1-4min, the stirring velocity that second segment stirs is 100-200r/min, churning time is 1-4min, the stirring velocity of the 3rd section of stirring is 10-50r/min, and churning time is 1-4min; Adopt slow, fast, slow syllogic to stir, be conducive to material and fully mix, avoid particle and material layering, and can avoid occurring stirring dead angle, mixing effect is good, is conducive to improve the quality of products.
The 3rd step: second step is mixed to material and put into twin screw extruder and carry out extruding pelletization; Pellet feeding section extrusion temperature is: 230-250 ℃, fluxing zone extrusion temperature is: 250-270 ℃, 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.Temperature to the each course of processing in product preparation process is strictly controlled, and guarantees the full and uniform fusion of material, and product light transmission is good, and flame retardant properties is high.
Preferably, in the described the first step, stirring velocity is 120-180r/min, and churning time is 2-3min.
Preferably, in described second step, the churning time that first paragraph stirs is 2min, and the churning time that second segment stirs is 2min, and the churning time of the 3rd section of stirring is 1min.
Preferably, in described the 3rd step, pellet feeding section extrusion temperature is: 235-245 ℃, fluxing zone extrusion temperature is: 255-265 ℃, 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, comprise the raw material of following component and mass percent: polycarbonate 94.8-99.5%, fire retardant A0.1-0.3%, fire retardant B0.1-3.5%, antioxidant A0.1-0.3%, antioxidant 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 processing step: the first step: fire retardant A, fire retardant B, oxidation inhibitor A, fire retardant B, lubricant, photostabilizer are put into homogenizer and stirred, and stirring velocity is 100-200r/min, and churning time is 2-4min; Second step: put into homogenizer together with the material that polycarbonate is mixed with the first step and carry out syllogic and stir evenly, the stirring velocity that first paragraph stirs is 20-50r/min, churning time is 1-4min, the stirring velocity that second segment stirs is 100-200r/min, churning time is 1-4min, the stirring velocity of the 3rd section of stirring is 10-50r/min, and churning time is 1-4min; The 3rd step: second step is mixed to material and put into twin screw extruder and carry out extruding pelletization; Pellet feeding section extrusion temperature is: 230-250 ℃, fluxing zone extrusion temperature is: 250-270 ℃, 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 advantages of light transmission and good flame resistance, can meet the requirement of outdoor lighting lampshade, and technique is simple, ripe, and production cost is low, is conducive to generally apply.
Advantage of the present invention has: (1) is keeping, under polycarbonate high flame retardant effect (2.0mm V0) prerequisite, having kept more than 90% high transmission rate of material.
(2) consumption of main flame retardant is less, and the shock resistance of the polycarbonate material making is up to 600-700, and IZOD notched Izod impact strength is high, and not easily broken when assembling product, structural strength is high, practical.
(3) auxiliary 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 making is constant in 10-11(ASTM D1238) between, the thermal stability of product is good, and mold temperature is moderate, effectively avoids product surface to occur scalelike mark, and quality product is high.
(5) flame retardant resistance of the product making is 2.0mm(V2, V0), flame retardant properties is high, and just matches with the thickness (2.0mm) of the light fixture outer cover of existing standard outdoor illumination requirement, is conducive to generally apply.
(6) the fluorescence burn-in test performance of the product making is good, at irradiation intensity 0.55W/M 2under 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 in reaching high light transmittance energy, and quality product is high, is applicable to being applied to outdoor lighting outer cover material, product excellent combination property.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated, and this is preferred embodiment of the present invention.
embodiment mono-.
A kind of high transmission rate of the present embodiment, high flame retardant polycarbonate material, comprise the raw material of following component and mass percent: 2805 bisphenol A polycarbonate of 99.5% Bayer AG, 0.1% sulfobenzide sulfonate, 0.1% bromination carbonate oligomer, 0.1% tricresyl phosphite (2,4-di-tert-butyl) ester, 0.1% β-(3,5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid, octadecanoic acid-2-(methylol of 0.1%)-2-[[(1-oxo octadecyl) oxygen base] methyl]-1,3-glyceryl ester.
Its preparation method is: the first step: the raw material of the above-mentioned mass percent proportioning beyond bisphenol A polycarbonate is put into homogenizer and stir, stirring velocity is 100r/min, and churning time is 4min; Second step: put into homogenizer together with the material that bisphenol A polycarbonate is mixed with the first step and carry out syllogic and stir evenly, the stirring velocity that first paragraph stirs is 20r/min, churning time is 4min, the stirring velocity that second segment stirs is 100r/min, churning time is 4min, the stirring velocity of the 3rd section of stirring is 10r/min, and churning time is 4min; The 3rd step: second step is mixed to material and put into twin screw extruder and carry out extruding pelletization; Pellet feeding section extrusion temperature is: 230 ℃, fluxing zone extrusion temperature is: 250 ℃, 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, have melting behaviour good, tensile strength is high, and elongation at break is greater than 80%, flexural strength is high, crooked elastic rate is high, and IZOD notched Izod impact strength is large, and heat-drawn wire is moderate, full light is crossed light rate and is reached more than 90%, fluorescence burn-in test performance is good, and product appearance transparency is high, the advantage that flame retardant properties is good.
embodiment bis-.
A kind of high transmission rate of the present embodiment, high flame retardant polycarbonate material, comprise the raw material of following component and mass percent: the bisphenol A polycarbonate of the 1250Z of 99.1% Di Ren company, 0.1% sulfobenzide sulfonate, 0.3% bromination carbonate oligomer, 0.1% tricresyl phosphite (2, 4-di-tert-butyl) ester, 0.1% β-(3, 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid, octadecanoic acid-2-(methylol of 0.2%)-2-[[(1-oxo octadecyl) oxygen base] methyl]-1, 3-glyceryl ester and 0.1% Octabenzone.
Its preparation method is: the first step: the raw material of the above-mentioned mass percent proportioning beyond bisphenol A polycarbonate is put into homogenizer and stir, stirring velocity is 140r/min, and churning time is 3min; Second step: put into homogenizer together with the material that bisphenol A polycarbonate is mixed with the first step and carry out syllogic and stir evenly, the stirring velocity that first paragraph stirs is 30r/min, churning time is 3min, the stirring velocity that second segment stirs is 140r/min, churning time is 3min, the stirring velocity of the 3rd section of stirring is 20r/min, and churning time is 3min; The 3rd step: second step is mixed to material and put into twin screw extruder and carry out extruding pelletization; Pellet feeding section extrusion temperature is: 240 ℃, fluxing zone extrusion temperature is: 260 ℃, melt conveying zone extrusion temperature is: 260 ℃, head temperature is: 250 ℃, the vacuum tightness that extruding pelletization adds man-hour is 0.7MPa.
embodiment tri-.
A kind of high transmission rate of the present embodiment, high flame retardant polycarbonate material, comprise the raw material of following component and mass percent: the bisphenol A polycarbonate of the 1201-10 of 98.6% the Dow Chemical Company, 0.2% sulfobenzide sulfonate, 0.7% bromination carbonate oligomer, 0.1% tricresyl phosphite (2, 4-di-tert-butyl) ester, 0.1% β-(3, 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid, octadecanoic acid-2-(methylol of 0.2%)-2-[[(1-oxo octadecyl) oxygen base] methyl]-1, 3-glyceryl ester and 0.1% Octabenzone.
Its preparation method is: the first step: the raw material of the above-mentioned mass percent proportioning beyond bisphenol A polycarbonate is put into homogenizer and stir, stirring velocity is 180r/min, and churning time is 3.5min; Second step: put into homogenizer together with the material that bisphenol A polycarbonate is mixed with the first step and carry out syllogic and stir evenly, the stirring velocity that first paragraph stirs is 40r/min, churning time is 2min, the stirring velocity that second segment stirs is 180r/min, churning time is 2min, the stirring velocity of the 3rd section of stirring is 30r/min, and churning time is 2min; The 3rd step: second step is mixed to material and put into twin screw extruder and carry out extruding pelletization; Pellet feeding section extrusion temperature is: 245 ℃, fluxing zone extrusion temperature is: 265 ℃, melt conveying zone extrusion temperature is: 265 ℃, head temperature is: 255 ℃, the vacuum tightness that extruding pelletization adds man-hour is 0.75MPa.
embodiment tetra-.
A kind of high transmission rate of the present embodiment, high flame retardant polycarbonate material, comprise the raw material of following component and mass percent: 2805 bisphenol A polycarbonate of 98.1% Bayer AG, 0.2% sulfobenzide sulfonate, 1.0% bromination carbonate oligomer, 0.1% tricresyl phosphite (2, 4-di-tert-butyl) ester, 0.1% β-(3, 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid, octadecanoic acid-2-(methylol of 0.2%)-2-[[(1-oxo octadecyl) oxygen base] methyl]-1, 3-glyceryl ester and 0.3% Octabenzone.
Its preparation method is: the first step: the raw material of the above-mentioned mass percent proportioning beyond bisphenol A polycarbonate is put into homogenizer and stir, stirring velocity is 200r/min, and churning time is 2min; Second step: put into homogenizer together with the material that bisphenol A polycarbonate is mixed with the first step and carry out syllogic and stir evenly, the stirring velocity that first paragraph stirs is 50r/min, churning time is 1min, the stirring velocity that second segment stirs is 200r/min, churning time is 1min, the stirring velocity of the 3rd section of stirring is 40r/min, and churning time is 1min; The 3rd step: second step is mixed to material and put into twin screw extruder and carry out extruding pelletization; Pellet feeding section extrusion temperature is: 250 ℃, fluxing zone extrusion temperature is: 270 ℃, 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 the present embodiment, high flame retardant polycarbonate material, comprise the raw material of following component and mass percent: the bisphenol A polycarbonate of the 1250Z of 97.6% Di Ren company, 0.2% sulfobenzide sulfonate, 1.4% bromination carbonate oligomer, 0.1% tricresyl phosphite (2, 4-di-tert-butyl) ester, 0.1% β-(3, 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid, octadecanoic acid-2-(methylol of 0.2%)-2-[[(1-oxo octadecyl) oxygen base] methyl]-1, 3-glyceryl ester and 0.4% Octabenzone.
Its preparation method is: the first step: the raw material of the above-mentioned mass percent proportioning beyond bisphenol A polycarbonate is put into homogenizer and stir, stirring velocity is 200r/min, and churning time is 2min; Second step: put into homogenizer together with the material that bisphenol A polycarbonate is mixed with the first step and carry out syllogic and stir evenly, the stirring velocity that first paragraph stirs is 50r/min, churning time is 1min, the stirring velocity that second segment stirs is 200r/min, churning time is 1min, the stirring velocity of the 3rd section of stirring is 50r/min, and churning time is 1min; The 3rd step: second step is mixed to material and put into twin screw extruder and carry out extruding pelletization; Pellet feeding section extrusion temperature is: 250 ℃, fluxing zone extrusion temperature is: 270 ℃, 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 the present embodiment, high flame retardant polycarbonate material, comprise the raw material of following component and mass percent: 2805 bisphenol A polycarbonate of 97.1% Bayer AG, 0.1% sulfobenzide sulfonate, 2.0% bromination carbonate oligomer, 0.1% tricresyl phosphite (2, 4-di-tert-butyl) ester, 0.1% β-(3, 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid, octadecanoic acid-2-(methylol of 0.1%)-2-[[(1-oxo octadecyl) oxygen base] methyl]-1, 3-glyceryl ester and 0.5% Octabenzone.
The performance of the preparation method of the present embodiment and the product of preparing is identical with embodiment mono-, repeats no more here.
embodiment seven.
A kind of high transmission rate of the present embodiment, high flame retardant polycarbonate material, comprise the raw material of following component and mass percent: the bisphenol A polycarbonate of the 1250Z of 95.6% Di Ren company, 0.3% sulfobenzide sulfonate, 3.0% bromination carbonate oligomer, 0.2% tricresyl phosphite (2, 4-di-tert-butyl) ester, 0.2% β-(3, 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid, octadecanoic acid-2-(methylol of 0.1%)-2-[[(1-oxo octadecyl) oxygen base] methyl]-1, 3-glyceryl ester and 0.6% Octabenzone.
The performance of the preparation method of the present embodiment and the product of preparing is identical with embodiment bis-, repeats no more here.
embodiment eight.
A kind of high transmission rate of the present embodiment, high flame retardant polycarbonate material, comprise the raw material of following component and mass percent: the bisphenol A polycarbonate of the 1201-10 of 94.8% the Dow Chemical Company, 0.3% sulfobenzide sulfonate, 3.5% bromination carbonate oligomer, 0.3% tricresyl phosphite (2, 4-di-tert-butyl) ester, 0.3% β-(3, 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid, octadecanoic acid-2-(methylol of 0.2%)-2-[[(1-oxo octadecyl) oxygen base] methyl]-1, 3-glyceryl ester and 0.6% Octabenzone.
The performance of the preparation method of the present embodiment and the product of preparing is identical with embodiment tri-, repeats no more here.
Below the each component of above-described embodiment one to embodiment eight and the list of mass percent thereof:
Sequence number Polycarbonate Fire retardant A Fire retardant B Antioxidant A Antioxidant 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 the properties test index of the polycarbonate material made of the component raw material of above-described embodiment one to embodiment eight:
Figure 833889DEST_PATH_IMAGE002
Can find out from the properties test 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 light rate, meet the requirement of outdoor lighting high brightness, be suitable for making outdoor lighting lampshade; The stable performance of fluorescence burn-in test, product is difficult for aging and yellow, and quality product is high, long service life; Fracture extensibility is large, IZOD notched Izod impact strength is high, and installation process is not fragile, practical.
Finally should be noted that; above embodiment is only in order to illustrate technical scheme of the present invention; but not limiting the scope of the invention; although the present invention has been done to explain with reference to preferred embodiment; those of ordinary skill in the art is to be understood that; can modify or be equal to replacement technical scheme of the present invention, and not depart from essence and the scope of technical solution of the present invention.

Claims (8)

1. high transmission rate, a 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%
Antioxidant A 0.1-0.3%
Antioxidant B 0.1-0.3%
Lubricant 0.1-0.2%
Photostabilizer 0-0.6%
Wherein, described polycarbonate is bisphenol A polycarbonate, and molecular weight is 26000-40000;
Wherein, described fire retardant A is sulfobenzide sulfonate; Described fire retardant B is bromination carbonate oligomer;
Wherein, described antioxidant A is tricresyl phosphite (2,4-di-tert-butyl) ester; Described antioxidant B is the positive octadecanol ester of β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid; The ratio of the mass percent of described antioxidant A and described antioxidant B is 1:1;
Wherein, described lubricant is octadecanoic acid-2-(methylol)-2-[[(1-oxo octadecyl) oxygen base] methyl]-1,3-glyceryl ester;
Wherein, described photostabilizer is Octabenzone;
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%
Antioxidant A 0.1-0.3%
Antioxidant 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%
Antioxidant A 0.1-0.2%
Antioxidant 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: described bisphenol A polycarbonate is Bayer AG 2805, the 1250Z of Di Ren company or the 1201-10 of the Dow Chemical Company.
5. the preparation method of a kind of high transmission rate described in any one, high flame retardant polycarbonate material in claim 1-4, is characterized in that: comprise following processing step:
The first step: fire retardant A, fire retardant B, oxidation inhibitor A, fire retardant B, lubricant, photostabilizer are put in homogenizer and stirred successively, and stirring velocity is 100-200r/min, and churning time is 2-4min;
Second step: put into homogenizer together with the material that polycarbonate is mixed with the first step and carry out syllogic and stir evenly, the stirring velocity that first paragraph stirs is 20-50r/min, churning time is 1-4min, the stirring velocity that second segment stirs is 100-200r/min, churning time is 1-4min, the stirring velocity of the 3rd section of stirring is 10-50r/min, and churning time is 1-4min;
The 3rd step: second step is mixed to material and put into twin screw extruder and carry out extruding pelletization; Pellet feeding section extrusion temperature is: 230-250 ℃, fluxing zone extrusion temperature is: 250-270 ℃, 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.
6. the preparation method of a kind of high transmission rate according to claim 5, high flame retardant polycarbonate material, is characterized in that: in the described the first step, stirring velocity is 120-180r/min, and churning time is 2-3min.
7. the preparation method of a kind of high transmission rate according to claim 5, high flame retardant polycarbonate material, it is characterized in that: in described second step, the churning time that first paragraph stirs is 2min, and the churning time that second segment stirs is 2min, and the churning time of the 3rd section of stirring is 1min.
8. the preparation method of a kind of high transmission rate according to claim 5, high flame retardant polycarbonate material, it is characterized in that: in described the 3rd step, pellet feeding section extrusion temperature is: 235-245 ℃, fluxing zone extrusion temperature is: 255-265 ℃, 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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