CN101851408A - A kind of halogen-free flame-retardant polycarbonate composition and preparation method thereof - Google Patents
A kind of halogen-free flame-retardant polycarbonate composition and preparation method thereof Download PDFInfo
- Publication number
- CN101851408A CN101851408A CN201010175493A CN201010175493A CN101851408A CN 101851408 A CN101851408 A CN 101851408A CN 201010175493 A CN201010175493 A CN 201010175493A CN 201010175493 A CN201010175493 A CN 201010175493A CN 101851408 A CN101851408 A CN 101851408A
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- halogen
- phosphorus
- retardant
- flame
- polycarbonate composition
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Links
- 239000004417 polycarbonate Substances 0.000 title claims abstract 16
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract 15
- 239000003063 flame retardant Substances 0.000 title claims abstract 15
- 239000000203 mixture Substances 0.000 title claims abstract 14
- 229920000515 polycarbonate Polymers 0.000 title claims abstract 14
- 238000002360 preparation method Methods 0.000 title claims abstract 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract 13
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract 13
- 239000011574 phosphorus Substances 0.000 claims abstract 13
- 239000003963 antioxidant agent Substances 0.000 claims abstract 4
- 230000003078 antioxidant effect Effects 0.000 claims abstract 4
- 239000003795 chemical substances by application Substances 0.000 claims abstract 4
- 238000004132 cross linking Methods 0.000 claims abstract 2
- 229910052736 halogen Inorganic materials 0.000 claims abstract 2
- 150000002367 halogens Chemical class 0.000 claims abstract 2
- 239000008188 pellet Substances 0.000 claims abstract 2
- 238000002156 mixing Methods 0.000 claims 2
- -1 polytetrafluoroethylene Polymers 0.000 claims 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims 2
- 239000002033 PVDF binder Substances 0.000 claims 1
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims 1
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- 238000001125 extrusion Methods 0.000 claims 1
- 239000000835 fiber Substances 0.000 claims 1
- 238000002844 melting Methods 0.000 claims 1
- 230000008018 melting Effects 0.000 claims 1
- 239000002530 phenolic antioxidant Substances 0.000 claims 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims 1
- 239000012994 photoredox catalyst Substances 0.000 abstract 1
Classifications
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
本发明涉及一种无卤阻燃聚碳酸酯组合物及其制备方法，属于阻燃技术领域。利用含磷的笼形或者梯形或者无规交联结构的低聚硅倍半氧烷作为阻燃剂阻燃PC，将聚碳酸酯、含磷低聚硅倍半氧烷、抗熔滴剂和抗氧化剂混合后通过双螺杆机熔融、混炼、挤出、冷却、切粒、干燥，得到无卤阻燃聚碳酸酯组合物粒料。含磷笼形或梯形或无规交联低聚硅倍半氧烷的结构通式为Tn(OH)m，T＝RSiO1.5-m/2n，R为R1、R2、R3或三者的任意组合，本发明采用含磷笼形或者梯形或者无规交联结构的低聚硅倍半氧烷为阻燃剂，其阻燃性强，热稳定性好，使所得的聚碳酸酯组合物在不含卤素同时具有较高的热变形温度、良好的阻燃性能和良好的机械性能。The invention relates to a halogen-free flame-retardant polycarbonate composition and a preparation method thereof, belonging to the field of flame-retardant technology. Using phosphorus-containing cage or trapezoidal or random cross-linked oligomeric silsesquioxane as a flame retardant to flame-retardant PC, polycarbonate, phosphorus-containing oligomeric silsesquioxane, anti-dropping agent and After the antioxidant is mixed, the mixture is melted, kneaded, extruded, cooled, pelletized and dried by a twin-screw machine to obtain pellets of the halogen-free flame-retardant polycarbonate composition. The general structural formula of phosphorus-containing cage or trapezoidal or random cross-linked oligosilsesquioxane is T n (OH) m , T=RSiO 1.5-m/2n , R is R1, R2, R3 or all three random combination,
The present invention adopts the oligomeric silsesquioxane of phosphorus-containing cage or trapezoid or random cross-linking structure as a flame retardant, which has strong flame retardancy and good thermal stability, so that the obtained polycarbonate composition does not contain Halogen also has a high heat distortion temperature, good flame retardancy and good mechanical properties.
Description
Technical field
The present invention relates to a kind of halogen-free flame-retardant polycarbonate composition and preparation method thereof, belong to the flame-retarded technology field.
Background technology
Polycarbonate (PC) engineering plastics are to use the fastest general engineering plastic of rate of growth, and itself has good thermostability and mechanical property.Polycarbonate itself is flammable, and have the band flame molten drop drip, following material ignites.Along with the raising that electronics, electric equipment products etc. require flame retardant properties, its flame-retardant modified research is more and more paid attention to.Fire retardant commonly used at present has halogenated flame retardant, phosphorus flame retardant etc.But because the problem of environmental pollution of halogenated flame retardant, increasing efficient halogen containing flame-retardant is disabled, especially in West Europe, developed country or areas such as Japan, North America.
Organophosphate is the halogen-free flame retardants that a class is widely used, and itself decomposition temperature is lower, though addition is PC to be had fire retardation preferably at 5%～10% o'clock, but can be very big when adding separately to the mechanical property infringement.
Cage type oligomer silasesquioxanes (polyhedral oligomeric silsesquioxanes, POSS, be also referred to as silicious sesquioxane) be a kind of hybrid inorganic-organic materials with three-dimensional cage structure of nano-scale, have the advantage of organic materials and inorganic materials simultaneously.Therefore, numerous areas such as POSS, catalyzer fire-retardant at polymkeric substance, printing, electrochemistry has a wide range of applications.For example, in the polymkeric substance flame retardant area, POSS can add in the polymkeric substance by multiple means such as blend, grafting, crosslinked and copolymerization, to improve thermostability, the oxidation-resistance of polymkeric substance, reduces the incendivity of compound.
Phosphorous its general structure of cage type oligomer silasesquioxanes is T among the present invention
n(OH)
m, T=R1SiO wherein
1.5-m/2nThe preparation method see that the patent No. is 201010128415.9 patent.
Summary of the invention
The objective of the invention is for the problem of environmental pollution that solves halogenated flame retardant and organophosphate decomposition temperature low and when adding separately to the big problem of mechanical property infringement, a kind of halogen-free flame-retardant polycarbonate composition and preparation method thereof is proposed.
The objective of the invention is to be achieved through the following technical solutions.
A kind of halogen-free flame-retardant polycarbonate composition of the present invention, the oligomer silasesquioxanes that utilizes phosphorated cage type or trapezoidal or random crosslinking structure is as fire retardant PC, in the total mass of halogen-free flame-retardant polycarbonate composition, the quality percentage composition of its each component is:
Polycarbonate 89%～98%
Phosphorous oligomer silasesquioxanes 1%～10%
Anti-molten drop agent 0.1%～0.5%
Antioxidant 0.4%～1.0%
The general structure of above-mentioned phosphorous oligomer silasesquioxanes is T
n(OH)
m, its structure has two classes:
1) phosphorous cage type oligomer silasesquioxanes: its general structure is T
n(OH)
m, T=RSiO wherein
1.5-m/2n, 4≤n≤12,0≤m≤4;
2) oligomer silasesquioxanes of phosphorous trapezoidal or random crosslinking: its general structure is T
n(OH)
m, T=RSiO wherein
1.5-m/2n, n 〉=4, m 〉=0;
T=RSiO wherein
1.5-m/2n, R is R1, R2, R3 or three's a arbitrary combination, R1 wherein, and the structural formula of R2 and R3 group is as follows:
Above-mentioned anti-molten drop agent is tetrafluoroethylene, polyvinylidene difluoride (PVDF), poly-hexafluoroethylene, poly-(tetrafluoroethylene-hexafluoroethylene), preferably has the fiber of formation ability, molecular-weight average is 1 * 10
5～2 * 10
7Tetrafluoroethylene;
Above-mentioned antioxidant is phenolic antioxidant 1010, phosphite ester kind antioxidant 168 or both mixtures.
The preparation method of a kind of halogen-free flame-retardant polycarbonate composition of the present invention, its concrete preparation process is:
After polycarbonate, phosphorous oligomer silasesquioxanes, anti-molten drop agent and antioxidant mixed, with mixture by the dual-screw-stem machine fusion, mixing, extrude, cooling, pelletizing, drying, obtain the halogen-free flame-retardant polycarbonate composition pellet.
In above-mentioned fusion, mixing, the extrusion, each zone temperatures of twin screw extruder should be 240～265 ℃; Drying temperature is 120 ℃.
The halogen-free flame-retardant polycarbonate composition pellet that obtains is passed through the injection moulding machine injection moulding, be used for using or test, each zone temperatures should be controlled at 250～275 ℃ during the injection moulding machine moulding.
Beneficial effect
It is fire retardant that the present invention adopts the oligomer silasesquioxanes of phosphorous cage type or trapezoidal or random crosslinking structure, its flame retardant resistance is strong, Heat stability is good, the polycarbonate compositions that makes gained does not have higher heat-drawn wire, good flame retardancy and a favorable mechanical performance simultaneously halogen-containing.
Embodiment
The invention will be further described below in conjunction with specific embodiment, but the present invention's scope required for protection is not limited to the related scope of embodiment.
Embodiment 1
With 97.3 parts of polycarbonate (trade mark PC2805, Bayer MaterialScience Tradings's product), after 2 parts of phosphorous cage type oligomer silasesquioxaness, 0.4 part of antioxidant 1010, the 0.3 part of tetrafluoroethylene dispersing and mixing, by the dual-screw-stem machine fusion, mixing, extrude, cooling, pelletizing, drying, obtain the halogen-free flame-retardant polycarbonate composition pellet; In fusion, mixing, the extrusion, each zone temperatures of twin screw extruder should be 240,250,260,265,255,245 ℃; Drying temperature is 120 ℃; Then the halogen-free flame-retardant polycarbonate composition pellet is passed through the injection moulding machine injection moulding, each zone temperatures should be controlled at 250,265,275,265 ℃ during the injection moulding machine moulding; Wherein the tetrafluoroethylene molecular-weight average is 3 * 10
5Phosphorous cage type oligomer silasesquioxanes is the mixture of A and B; Wherein the structural formula of A is T
8, T=R1SiO wherein
1.5, its structural formula is seen formula (1), the structural formula of B is T
9(OH)
1, T=R1SiO wherein
13/9, its structural formula is seen formula (2):
Embodiment 2
With 95.1 parts of polycarbonate (trade mark PC2805, Bayer MaterialScience Tradings's product), after 4 parts of phosphorous cage type oligomer silasesquioxaness, 168,0.4 part of antioxidant 1010 of 0.2 part of oxidation inhibitor, the 0.3 part of tetrafluoroethylene dispersing and mixing, by the dual-screw-stem machine fusion, mixing, extrude, cooling, pelletizing, drying, obtain the halogen-free flame-retardant polycarbonate composition pellet; In fusion, mixing, the extrusion, each zone temperatures of twin screw extruder should be 240,250,260,265,255,245 ℃; Drying temperature is 120 ℃; Then the halogen-free flame-retardant polycarbonate composition pellet is passed through the injection moulding machine injection moulding, each zone temperatures should be controlled at 250,265,275,265 ℃ during the injection moulding machine moulding; Wherein the tetrafluoroethylene molecular-weight average is 3 * 10
5Phosphorous cage type oligomer silasesquioxanes is the mixture of A and B; Wherein the structural formula of A is T
8, T=R1SiO wherein
1.5, the structural formula of B is T
9(OH)
1, T=R1SiO wherein
13/9
Embodiment 3
With 93.1 parts of polycarbonate (trade mark PC2805, Bayer MaterialScience Tradings's product), after 6 parts of phosphorous cage type oligomer silasesquioxaness, 168,0.4 part of antioxidant 1010 of 0.2 part of oxidation inhibitor, the 0.3 part of tetrafluoroethylene dispersing and mixing, by the dual-screw-stem machine fusion, mixing, extrude, cooling, pelletizing, drying, obtain the halogen-free flame-retardant polycarbonate composition pellet; In fusion, mixing, the extrusion, each zone temperatures of twin screw extruder should be 240,250,260,265,255,245 ℃; Drying temperature is 120 ℃; Then the halogen-free flame-retardant polycarbonate composition pellet is passed through the injection moulding machine injection moulding, each zone temperatures should be controlled at 250,265,275,265 ℃ during the injection moulding machine moulding; Wherein the tetrafluoroethylene molecular-weight average is 3 * 10
5Phosphorous cage type oligomer silasesquioxanes is the mixture of A and B; Wherein the structural formula of A is T
8, T=R1SiO wherein
1.5, the structural formula of B is T
9(OH)
1, T=R1SiO wherein
13/9
Embodiment 4
With 93.3 parts of polycarbonate (trade mark PC2805, Bayer MaterialScience Tradings's product), 6 parts contain trapezoidal oligomer silasesquioxanes, 168,0.3 part of tetrafluoroethylene dispersing and mixing of 0.4 part of oxidation inhibitor after, by the dual-screw-stem machine fusion, mixing, extrude, cooling, pelletizing, drying, obtain the halogen-free flame-retardant polycarbonate composition pellet; In fusion, mixing, the extrusion, each zone temperatures of twin screw extruder should be 240,250,260,265,255,245 ℃; Drying temperature is 120 ℃; Then the halogen-free flame-retardant polycarbonate composition pellet is passed through the injection moulding machine injection moulding, each zone temperatures should be controlled at 250,265,275,265 ℃ during the injection moulding machine moulding; Wherein the tetrafluoroethylene molecular-weight average is 3 * 10
5Phosphorous trapezoidal oligomer silasesquioxanes is T
8(OH)
4, T=R1SiO wherein
1.25, its structural formula is seen formula (3):
Embodiment 1, embodiment 2, embodiment 3 and embodiment 4 prepared compositions are injection molded into the required batten of test according to standard size.
Standard testing heat-drawn wire according to GB 1634-2004; Standard testing tensile property according to ASTM D638; Standard testing bending property according to ASTM D790; Standard according to ISBN 0762900822 is carried out the flammable experiment of UL-94 to batten.
Pure PC and each example composition The performance test results are as shown in table 1:
The pure PC of table 1. and each example composition The performance test results
| Performance | Pure PC | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Heat-drawn wire (℃) | ??136.3 | ??133.0 | ??131.1 | ??128.5 | ??127.8 |
| Tensile strength (MPa) | ??61.2 | ??63.8 | ??66.5 | ??67.5 | ??68.0 |
| Elongation at break (%) | ??120 | ??102 | ??64 | ??16 | ??18 |
| Flexural strength (MPa) | ??87.5 | ??91.1 | ??91.7 | ??94.5 | ??93.7 |
| Modulus in flexure (MPa) | ??2298 | ??2402 | ??2445 | ??2548 | ??2506 |
| 3.2mm batten burning grade | ??V-2 | ??V-2 | ??V-0 | ??V-0 | ??V-0 |
Claims (5)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101754934A CN101851408B (en) | 2010-05-14 | 2010-05-14 | Halogen-free flame-retardant polycarbonate composition and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101754934A CN101851408B (en) | 2010-05-14 | 2010-05-14 | Halogen-free flame-retardant polycarbonate composition and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN101851408A true CN101851408A (en) | 2010-10-06 |
| CN101851408B CN101851408B (en) | 2012-04-18 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102206401A (en) * | 2011-04-14 | 2011-10-05 | 北京理工大学 | Halogen-free flame-retardant epoxy resin composition and preparation method thereof |
| CN104403289A (en) * | 2014-11-06 | 2015-03-11 | 北京理工阻燃科技有限公司 | Halogen-free flame-retardant polycarbonate composition and preparation method thereof |
| CN106700471A (en) * | 2016-12-19 | 2017-05-24 | 合肥会通新材料有限公司 | Chemical-resisting inflaming-retarding polycarbonate material and preparation method thereof |
| CN109233238A (en) * | 2018-08-30 | 2019-01-18 | 北京理工大学 | A kind of Polyhedral oligomeric silsesquioxane fire-retardant polycarbonate and its preparation method and application |
| CN110218434A (en) * | 2019-07-12 | 2019-09-10 | 广州爱奇实业有限公司 | A kind of flame-retardant polycarbonate material and its preparation method and application |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5081202A (en) * | 1989-11-17 | 1992-01-14 | Mitsubishi Denki Kabushiki Kaisha | High purity phenyl silicone ladder polymer and method for producing the same |
| CN100513411C (en) * | 2007-01-19 | 2009-07-15 | 华南理工大学 | Double-ring cage shape substituted silsesquioxane and its preparation method and uses |
| CN101519529A (en) * | 2009-03-26 | 2009-09-02 | 上海交通大学 | Polycarbonate composition and preparation method thereof |
-
2010
- 2010-05-14 CN CN2010101754934A patent/CN101851408B/en active Active
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102206401A (en) * | 2011-04-14 | 2011-10-05 | 北京理工大学 | Halogen-free flame-retardant epoxy resin composition and preparation method thereof |
| CN104403289A (en) * | 2014-11-06 | 2015-03-11 | 北京理工阻燃科技有限公司 | Halogen-free flame-retardant polycarbonate composition and preparation method thereof |
| CN104403289B (en) * | 2014-11-06 | 2016-05-11 | 北京理工阻燃科技有限公司 | A kind of halogen-free flame-retardant polycarbonate composition and preparation method |
| CN106700471A (en) * | 2016-12-19 | 2017-05-24 | 合肥会通新材料有限公司 | Chemical-resisting inflaming-retarding polycarbonate material and preparation method thereof |
| CN109233238A (en) * | 2018-08-30 | 2019-01-18 | 北京理工大学 | A kind of Polyhedral oligomeric silsesquioxane fire-retardant polycarbonate and its preparation method and application |
| CN110218434A (en) * | 2019-07-12 | 2019-09-10 | 广州爱奇实业有限公司 | A kind of flame-retardant polycarbonate material and its preparation method and application |
| CN110218434B (en) * | 2019-07-12 | 2021-08-27 | 广州爱奇实业有限公司 | Flame-retardant polycarbonate material and preparation method and application thereof |
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| CN101851408B (en) | 2012-04-18 |
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Owner name: BEIJING POLYTECHNIC FLAME RETARDANT TECHNOLOGY CO. Free format text: FORMER OWNER: BEIJING LIGONG UNIVERSITY Effective date: 20140402 |
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Effective date of registration: 20140402 Address after: 100081, Beijing, Zhongguancun Haidian District South Street No. 2, 5 District, 683, three, 307 Patentee after: BEIJING LIGONG FLAME RETARDATION TECHNOLOGY Co.,Ltd. Address before: 100081 No. 5, Zhongguancun South Street, Haidian District, Beijing Patentee before: BEIJING INSTITUTE OF TECHNOLOGY |