CN102079857B - Halogen-free flame-retardant polycarbonate (PC) composition and preparation method thereof - Google Patents
Halogen-free flame-retardant polycarbonate (PC) composition and preparation method thereof Download PDFInfo
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- CN102079857B CN102079857B CN2010106023206A CN201010602320A CN102079857B CN 102079857 B CN102079857 B CN 102079857B CN 2010106023206 A CN2010106023206 A CN 2010106023206A CN 201010602320 A CN201010602320 A CN 201010602320A CN 102079857 B CN102079857 B CN 102079857B
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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
- B29C48/78—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
- B29C2948/9258—Velocity
- B29C2948/9259—Angular velocity
-
- 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
- B29C2948/92885—Screw or gear
-
- 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
Abstract
The invention discloses a halogen-free flame-retardant polycarbonate (PC) composition and a preparation method thereof, which belong to a PC composition. The composition comprises the following components in percentage by weight: PC, regenerated PC, a toughening agent, a halogen-free flame retardant, a composite antioxidant, a fluorine-containing anti-dripping agent, a compatilizer, a lubricant and a dispersant. The preparation method comprises the following steps of: adding the components into a high-speed stirrer in turn and stirring fully and uniformly; and adding the mixture into a double screw extruder, performing melt extrusion, cooling and pelletizing so as to obtain the halogen-free flame-retardant PC composition. The halogen-free flame-retardant PC composition fully reaches the 1.6 mmV-0 standard of flame retardance UL-94, and has performance which is equivalent to that of a reference compound. Due to the application of the regenerated PC, the halogen-free flame-retardant PC composition has performance which is equivalent to that of the reference compound, low processing temperature and higher flowability and is easy for injection molding, and composition cost is lowered greatly.
Description
Technical field
The present invention relates to polycarbonate compositions, specifically is a kind of halogen-free flame retardant PC composition and method of making the same.
Background technology
Polycarbonate (PC) is a kind of thermoplastic engineering plastic of excellent combination property, has outstanding shock resistance, excellent mechanical property and flame retardant resistance.Flame retardant rating is UL94-V-2.But, there is hot melts to drip during still incendivity, and burning, material catches fire near causing easily, is difficult to satisfy the fire-retardant fireproof requirement.Therefore, in practical application, to carry out fire-retardant finish to PC.Yet can emit deleterious hydrogen halide and a large amount of smog during the halogen containing flame-retardant material combustion, even produce some carcinogenic substances, have a strong impact on the safety of people's lives and properties.So, along with society to the particular requirement of the environmental requirement of material and Application Areas to material, the feature of environmental protection of the flame retardant properties of engineering plastics compsn receives people's attention day by day.Halogen-free flame retardant PC is used for the communication appliance field then becomes developing focus.Chinese patent CN101591468A and Chinese patent CN101735585A disclose halogen-free flame retardant PC/ABS Alloy And Preparation Method.Above patent, in order to realize good flame-retardant effect, the large usage quantity of its fire retardant brings the PC performance to reduce for fear of heavy dose of fire retardant simultaneously, and it adopts the consumption that increases other auxiliary agent to guarantee composition properties.Owing to the particular requirement of electrical equipment aspect, regeneration PC material also is not used in the parts of making electrical equipment, telecommunication aspect, so the raw materials cost of these parts is relatively more expensive in addition.Though the CN101735585A patent discloses the PC that uses two kinds of different melting index, be not to use regenerated PC material, can not reduce cost significantly.
Summary of the invention
The objective of the invention is deficiency, and a kind of halogen-free flame retardant PC composition and method of making the same of a kind of easy processing, environmental protection, good flame resistance, mechanical property excellence is provided to prior art.
Another purpose of invention is not require that all performances of compsn of the present invention all are best; But make full use of regeneration PC material resources; Prepare excellent combination property, can satisfy the cheap relatively a kind of halogen-free flame retardant PC compsn of cost of electrical equipment, telecommunication parts working conditions.
Above-mentioned purpose of the present invention realizes through following technical scheme.
The present invention includes following components in weight percentage:
Polycarbonate 30-80%,
Recycled polycarbonate 14-70%,
Toughner 3-10%,
Halogen-free flame retardants 5-10%,
Composite antioxidant 0.2-0.5%,
Fluorine-containing anti-dripping agent 0.1-1.0%,
Compatilizer 3-10%,
Lubricant 0.1-0.7%,
Dispersion agent 0.1-0.2%.
Further comprise following weight percent component:
Polycarbonate: 30-65%,
Recycled polycarbonate: 14-50%,
Toughner: 5-6%,
Halogen-free flame retardants: 7-8%,
Composite antioxidant: 0.3-0.4%,
Fluorine-containing anti-dripping agent: 0.1-0.7%,
Compatilizer: 5-7%,
Lubricant: 0.1-0.7%,
Dispersion agent: 0.15-0.2%.
Preparing method of the present invention is following:
1. materials such as PC, regeneration PC, toughner, halogen-free flame retardants, composite antioxidant, fluorine-containing anti-dripping agent, compatilizer, lubricant, dispersion agent are added in the impeller successively, under 300-500 rev/min rotating speed, mixed 3-5 minute;
2. said mixture is added in the twin screw extruder, through melt extrude, cooling, pelletizing both obtained the halogen-free flame retardant PC compsn.
Its complete processing is following: twin screw extruder feeding section temperature is 180 ℃-225 ℃, and the fluxing zone temperature is 235 ℃-245 ℃, and the homogenizing zone temperature is 230 ℃-240 ℃, 215 ℃-230 ℃ of head temperatures.Screw speed 200-400rpm.
Said polycarbonate resin is selected all new resins in the 10-20g/10min scope of melting index for use.
Said recycled polycarbonate is corner blanking and unacceptable product in producing, reclaims continued and uses.Its melting index is 12-35g/10min.
Said toughner is selected from the raw materials such as acrylic acid esters co-polymer of multipolymer (ACR) and methacrylate butadi ene styrene copolymer (MBS) and nucleocapsid structure of TEB 3K and propenoate of acrylonitrile-butadiene-phenylethylene multipolymer (ABS), nucleocapsid structure any one or a few.
Said halogen-free flame retardants is selected from any one or a few in Sulfonates fire retardant and the aromatic phosphoric ester class halogen-free flame retardants.
Said composite antioxidant is the mixture of Hinered phenols primary antioxidant and phosphorous acid esters auxiliary anti-oxidant.
Said fluorine-containing anti-dripping agent is for being the fluoropolymers anti-dripping agent on basis with Fluroplast-4, and its particle diameter is 500um, and density is 2.165g/cm
3
Said compatilizer is the auxiliary agent of esters of acrylic acid, and plastic material is had the shock resistance of improvement and makes each composition of polyblend compatible performance easily.
Said lubricant is a silicone.Said dispersion agent is a white oil.
The present invention does not use the new resin of the little PC of melting index; And select the resin of melting index in the 10-20g/10min scope for use; As Bayer A.G 2805,2807, LG-DOW 201-15,201-10, any one in Saudi Arabia 141R, the Russian 010U resin improved processing characteristics like this on the basis that guarantees quality product; Reduce the usage quantity of auxiliary agent, also reduced processing temperature simultaneously.The regenerate melting index of PC of the present invention is 12-35g/10min.Guarantee that like this these two kinds of materials can merge preferably.
Said composite antioxidant is that commercially available producer is with Hinered phenols primary antioxidant and the mixed a kind of composite antioxidant got ready of phosphorous acid esters auxiliary anti-oxidant.
What adopt among the lubricant embodiment of the present invention is silicone, both can reduce the materials flow that adds man-hour and the friction of barrel, can increase flame retardant effect again.
Advantage of the present invention and positively effect are: compsn of the present invention adopts halogen-free flame retardants, and consumption is few in fire retardant of the same type, can put out certainly during burning, do not have drippage, abundant carbon-coating is arranged, and good flame retardation effect meets the ROHS of European Union standard.The halogen-free flame retardants that adopts is environmentally friendly, belongs to environmentfriendly products.Though the present invention's auxiliary dosage is few,, improved the processing characteristics and the various mechanical property of compsn through the prescription screening.Make processing temperature lower, good fluidity is prone to processing, and the high comprehensive performance of the finished product can reach the performance of the fire retardation PC compsn of finding report.In addition, the present invention utilizes blanking of PC corner and the unacceptable product in the production to carry out the reclaiming product, makes full use of renewable resource, has both practiced thrift the raw material and the energy, reduces the pollution to environment, has reduced cost again.When regeneration PC raw material reaches 50% when above of PC resin total amount, its performance can also be suitable with reference substance.Flame retardant properties can reach the standard of UL-94 1.6mm V-0 fully, and processing temperature is low, and is mobile better, is prone to injection moulding, and can significantly reduces the compsn cost.The present invention has important economic benefit, social benefit and ecological benefits.Compsn of the present invention can be used for preparing the parts of electrical equipment, telecommunication industry, can satisfy the user demand of these products.
Embodiment
Further specify the present invention through embodiment below.Below each prescription adopts all is weight percent.All changes of in technical scope of the present invention, being done are all in protection scope of the present invention.
The prescription of embodiment 1-4 is seen table 1.
Material choice:
1, the PC resin is selected LG-DOW 201-15 for use, and its melting index is that to select melting index for use be the material of 13-15g/10min for 15g/10min, PC reworked material.
2, toughner is selected homemade ABS-0215A for use.
3, halogen-free flame retardants is selected homemade aromatic phosphoric ester based flame retardant PX-220 for use.
4, composite antioxidant is selected homemade B-215 for use.
5, fluorine-containing anti-dripping agent is selected the TF-1645 of Minnesota Mining and Manufacturing Company for use.
6, compatilizer is selected the auxiliary agent CMPC5015 of homemade esters of acrylic acid for use.
7, lubricant is selected homemade silicone GM-100 for use.
8, dispersion agent is selected homemade 70N type white oil for use.
Halogen-free flame retardant PC compsn of the present invention adopts iso standard to detect.In order to compare with existing halogen-free flame retardant PC compsn, the halogen-free flame retardant PC composition material that is widely used in making telecommunication, electrical component at present that will buy from market carries out same detection as reference substance.Concrete performance data is seen table 2.
Table 1 embodiment 1-4 prescription
The preparation method:
1. materials such as PC, regeneration PC, toughner, halogen-free flame retardants, composite antioxidant, anti-dripping agent, compatilizer, lubricant, dispersion agent are added in the impeller successively, under 300-500 rev/min rotating speed, mixed 3-5 minute;
2. said mixture is added in the twin screw extruder, through melt extrude, cooling, pelletizing both obtained the halogen-free flame retardant PC compsn.
Expressing technique is following: twin screw extruder feeding section temperature is 180 ℃-225 ℃, and the fluxing zone temperature is 235 ℃-245 ℃, and the homogenizing zone temperature is 230 ℃-240 ℃, 215 ℃-230 ℃ of head temperatures; Screw speed 250-300rpm.
The Performance Detection data of table 2 embodiment 1-4
Claims (9)
1. halogen-free flame retardant PC compsn is characterized in that: comprise following components in weight percentage:
Polycarbonate: 30-65%,
Recycled polycarbonate: 14-50%,
Toughner: 5-6%,
Halogen-free flame retardants: 7-8%,
Composite antioxidant: 0.3-0.4%,
Fluorine-containing anti-dripping agent: 0.1-0.7%,
Compatilizer: 5-7%,
Lubricant: 0.1-0.7%,
Dispersion agent: 0.15-0.2%.
2. a kind of halogen-free flame retardant PC compsn according to claim 1 is characterized in that: the melting index of said polycarbonate is 10-20g/10min, and the melting index of recycled polycarbonate is 12-35g/10min.
3. a kind of halogen-free flame retardant PC compsn according to claim 2; It is characterized in that: said toughner is selected from the TEB 3K of acrylonitrile-butadiene-styrene copolymer, methacrylate butadi ene styrene copolymer, nucleocapsid structure and the multipolymer of propenoate, in the acrylic acid esters co-polymer of nucleocapsid structure any one or a few.
4. a kind of halogen-free flame retardant PC compsn according to claim 1 is characterized in that: said halogen-free flame retardants is selected from one or more in aromatic sulphonate and the aromatic phosphoric ester based flame retardant.
5. a kind of halogen-free flame retardant PC compsn according to claim 1 is characterized in that: said composite antioxidant is the compound thing of Hinered phenols primary antioxidant and phosphorous acid esters auxiliary anti-oxidant.
6. a kind of halogen-free flame retardant PC compsn according to claim 1 is characterized in that: said fluorine-containing anti-dripping agent is that particle diameter is 500 μ m, and density is 2.165g/cm
3With Fluroplast-4 be the basis the fluoropolymer anti-dripping agent.
7. a kind of halogen-free flame retardant PC compsn according to claim 1 is characterized in that: said compatilizer is an acrylic ester modifier.
8. a kind of halogen-free flame retardant PC compsn according to claim 1 is characterized in that: said lubricant is a silicone; Dispersion agent is a white oil.
9. one kind prepares the described a kind of halogen-free flame retardant PC method for compositions of claim 1:
1. materials such as PC resin, regeneration PC resin, toughner, halogen-free flame retardants, composite antioxidant, fluorine-containing anti-dripping agent, compatilizer, lubricant, dispersion agent are added in the impeller successively, under 300-500 rev/min rotating speed, mixed 3-5 minute,
2. said mixture is added twin screw extruder, through melt extrude, cooling, pelletizing promptly obtain the halogen-free flame retardant PC compsn; Complete processing is following: twin screw extruder feeding section temperature is 180-225 ℃, and the fluxing zone temperature is 235 ℃-245 ℃, and the homogenizing zone temperature is 230 ℃-240 ℃, 215 ℃-230 ℃ of head temperatures, screw speed 200-400rpm.
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| CN2010106023206A CN102079857B (en) | 2010-12-23 | 2010-12-23 | Halogen-free flame-retardant polycarbonate (PC) composition and preparation method thereof |
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| CN2010106023206A CN102079857B (en) | 2010-12-23 | 2010-12-23 | Halogen-free flame-retardant polycarbonate (PC) composition and preparation method thereof |
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| CN102079857B true CN102079857B (en) | 2012-03-28 |
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Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102311626B (en) * | 2011-07-06 | 2012-08-15 | 惠州市昌亿科技股份有限公司 | Polycarbonate/glass fiber alloy, preparation method and application thereof |
| CN102311610B (en) * | 2011-07-06 | 2012-09-05 | 惠州市昌亿科技股份有限公司 | Acrylonitrile-butadiene-styrene (ABS) composite material used for housing of intelligent water meter and preparation method thereof |
| CN102417704A (en) * | 2011-10-10 | 2012-04-18 | 福建奥峰科技有限公司 | Weather-resistant flame-retardant polycarbonate (PC) composition, and preparation method and application thereof |
| CN102558815A (en) * | 2011-12-17 | 2012-07-11 | 铜陵市新泰电容电器有限责任公司 | Modified polycarbonate material for processing of shell of capacitor of locomotive |
| CN102558814A (en) * | 2011-12-17 | 2012-07-11 | 铜陵市新泰电容电器有限责任公司 | Modified polymeric carbon ester material for preparing capacitor housing |
| CN102850757A (en) * | 2012-09-21 | 2013-01-02 | 常熟市凯力达蜂窝包装材料有限公司 | Transparent polycarbonate alloy material |
| CN103421295A (en) * | 2013-08-23 | 2013-12-04 | 韩清洁 | High flame-retardant recycled plastic for production of bullet train seats and preparation method thereof |
| CN106349676B (en) * | 2016-08-31 | 2018-10-23 | 广州合成材料研究院有限公司 | A kind of halogen-free flame retardant PC and preparation method thereof |
| CN106751662A (en) * | 2016-12-12 | 2017-05-31 | 广东威林工程塑料股份有限公司 | A kind of weather-proof, high glaze and phosphate halogen-free flame retardant PC/AES alloys and preparation method thereof |
| CN106751661A (en) * | 2016-12-12 | 2017-05-31 | 广东威林工程塑料股份有限公司 | A kind of low cost, HI high impact, high glaze and halogen-free and flame-retardant polycarbonate material and preparation method thereof |
| CN109111715A (en) * | 2018-07-30 | 2019-01-01 | 上海众力投资发展有限公司 | A kind of halogen-free toughening polycarbafil material and its preparation method and application |
| CN114249898B (en) * | 2021-12-16 | 2023-05-26 | 宁波坚锋新材料有限公司 | Modified organosilicon flame retardant and application thereof in recycling polycarbonate |
| CN115304900B (en) * | 2022-07-25 | 2023-11-10 | 宁波坚锋新材料有限公司 | Flame-retardant regenerated polycarbonate material and preparation method thereof |
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| CN101709142A (en) * | 2009-11-13 | 2010-05-19 | 北京化工大学 | High-toughness halogen-free flame-retardanting reclaimed polycarbonate compound and preparation method thereof |
| CN101759976A (en) * | 2008-11-21 | 2010-06-30 | 上海普利特复合材料股份有限公司 | Special polycarbonate/acrylonitrile-butadiene-styrene(PC/ABS) alloy material for notebook computer shell |
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| CN101389696B (en) * | 2006-01-06 | 2012-05-30 | 苏普雷斯塔有限责任公司 | Halogen-free flame retardant compositions, thermoplastic compositions comprising the same and methods of producing the compositions |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101759976A (en) * | 2008-11-21 | 2010-06-30 | 上海普利特复合材料股份有限公司 | Special polycarbonate/acrylonitrile-butadiene-styrene(PC/ABS) alloy material for notebook computer shell |
| CN101709142A (en) * | 2009-11-13 | 2010-05-19 | 北京化工大学 | High-toughness halogen-free flame-retardanting reclaimed polycarbonate compound and preparation method thereof |
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Denomination of invention: Halogen-free flame-retardant polycarbonate (PC) composition and preparation method thereof Effective date of registration: 20130118 Granted publication date: 20120328 Pledgee: Tianjin TEDA Small Enterprise Credit Guarantee Center Pledgor: Tianjin Guofeng Mold Co., Ltd. Registration number: 2013990000041 |
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