CN107880510A - A kind of activeness and quietness halogen-free and flame-retardant polycarbonate material and preparation method thereof - Google Patents

A kind of activeness and quietness halogen-free and flame-retardant polycarbonate material and preparation method thereof Download PDF

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Publication number
CN107880510A
CN107880510A CN201710999295.1A CN201710999295A CN107880510A CN 107880510 A CN107880510 A CN 107880510A CN 201710999295 A CN201710999295 A CN 201710999295A CN 107880510 A CN107880510 A CN 107880510A
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China
Prior art keywords
parts
free
toughener
halogen
flame
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CN201710999295.1A
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Chinese (zh)
Inventor
周健
杨菁菁
周仕龙
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Jiangsu University of Technology
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Jiangsu University of Technology
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Priority to CN201710999295.1A priority Critical patent/CN107880510A/en
Publication of CN107880510A publication Critical patent/CN107880510A/en
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00—Making granules
    • B29B9/02—Making granules by dividing preformed material
    • B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
    • C08J5/043—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with glass fibres
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2369/00—Characterised by the use of polycarbonates; Derivatives of polycarbonates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2451/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2451/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
    • C08J2451/08—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/02—Flame or fire retardant/resistant
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/22—Halogen free composition

Abstract

The invention discloses a kind of activeness and quietness halogen-free and flame-retardant polycarbonate material and preparation method thereof, the enhanced halogen-free and flame-retardant polycarbonate is made up of following components in parts by weight：100 parts of polycarbonate resin, fire retardant 0.04~0.15,0.1~0.4 part of composite antioxidant, 5~30 parts of reinforcing agent, 2~8 parts of toughener.The preparation method of the material is：Weigh the polycarbonate resin through drying process, fire retardant, composite antioxidant and toughener and pour into the mixing of mixer high speed, mixed material is sent to melting extrusion in double screw extruder, simultaneously long glass fibres is added in extruder waist exhaust outlet, the billot die head pelletizing extruded and water cooling, activeness and quietness halogen-free and flame-retardant polycarbonate material is produced by drying process.

Description

A kind of activeness and quietness halogen-free and flame-retardant polycarbonate material and preparation method thereof
Technical field
The present invention relates to a kind of high polymer material and preparation method thereof, and in particular to a kind of poly- carbon of activeness and quietness halogen-free flameproof Acid esters material and preparation method thereof.
Background technology
Makrolon (PC) is a kind of thermoplastic engineering plastic of excellent comprehensive performance, has prominent impact resistance, Creep resistance and dimensional stability, it is heat-resisting, water absorption rate is low, nontoxic, dielectric properties are excellent, but it is due to molecular structure reason, poly- carbon Acid esters exists in forming process is also easy to produce stress cracking phenomenon, and modified in addition fire retardant, its comprehensive mechanical property It can drastically decline, influence the engineer applied of makrolon.
The present invention is used cooperatively using reinforcing agent and toughener, is remarkably improved the synthesis mechanical property of fire-retardant polycarbonate Can, meet specific application area applies needs.
The content of the invention
An object of the present invention is to solve the above problems, there is provided one kind has application method easy, flexible, can meet The production of application-specific requirement, while there is the simple activeness and quietness of preferable mechanical property, heat resistance, production process Halogen-free and flame-retardant polycarbonate material.
Another object of the present invention is to provide the preparation method of above-mentioned activeness and quietness halogen-free and flame-retardant polycarbonate material.
Claimed activeness and quietness halogen-free and flame-retardant polycarbonate material, is made up of following components in parts by weight： 100 parts of polycarbonate resin, fire retardant 0.04~0.15,0.1~0.4 part of composite antioxidant, 5~30 parts of reinforcing agent, toughener 2 ~8 parts.
Preferable makrolon material, is made up of following components in parts by weight：100 parts of polycarbonate resin, fire retardant 0.05,0.4 part of composite antioxidant, 18 parts of reinforcing agent, 6 parts of toughener.
Preferable makrolon material, is made up of following components in parts by weight：100 parts of polycarbonate resin, fire retardant 0.05,0.4 part of composite antioxidant, 22 parts of reinforcing agent, 6 parts of toughener.
The preferable polycarbonate resin is middle viscosity or the high viscosity makrolon of bisphenol-A class.Described in preferable Fire retardant is perfluorobutyl potassium sulfonate；Preferable composite antioxidant by antioxidant 1010, irgasfos 168 according to 1: 3 weight ratio Composition.Preferable reinforcing agent is alkali-free long glass fibres.Preferable toughener is using crosslink propylene acid esters or organosilicon as core, is connect Branch methyl methacrylate is the compound of shell.
The preparation method of makrolon material of the present invention, comprises the following steps：
(1) polycarbonate resin through drying process, fire retardant, composite antioxidant and toughener will be weighed according to formula to fall Enter mixer high speed and mix 5~6min, discharging, obtain mixed material；
(2) mixed material obtained by step (1) is sent to melting extrusion in double screw extruder, while in extruder machine Exhaust outlet addition long glass fibres, the billot die head pelletizing extruded and water cooling, enhancing is produced by drying process in the middle part of body Toughened halogen-free flame-retardant makrolon material.
It is preferred that step (2) in the temperature in each area of double screw extruder be：T1=135~145 DEG C, T2=225~235 DEG C, T3=255~265 DEG C, T4=260~270 DEG C, T5=270~280 DEG C, T6=280~290 DEG C, T7=275~285 DEG C, T8= 260~270 DEG C, T9=250~260 DEG C, TMould=250~260 DEG C.
It is preferred that step (2) in the temperature in each area of double screw extruder be：T1=140 DEG C, T2=230 DEG C, T3=260 DEG C, T4=265 DEG C, T5=275 DEG C, T6=285 DEG C, T7=280 DEG C, T8=275 DEG C, T9=255 DEG C, TMould=255 DEG C.
It is preferred that step (1) in weigh the polycarbonate resin through drying process, fire retardant, composite antioxidant and toughener Pour into mixer high speed mixing 6min.
The good effect that the present invention has：
1. the activeness and quietness halogen-free and flame-retardant polycarbonate material of the present invention uses alkali-free long glass fiber reinforced makrolon to increase Strong agent has advantages below：
(1) good fire-retardant polycarbonate enhancing effect can be obtained and prevent stress cracking resistance；
(2) heat distortion temperature of fire-retardant polycarbonate is effectively improved.
2. the activeness and quietness halogen-free and flame-retardant polycarbonate material of the present invention is used using crosslink propylene acid esters or organosilicon as core, Grafted methacrylic acid methyl esters is that the compound of shell is toughener, ensure that halogen-free and flame-retardant polycarbonate material has and preferably increases Tough effect and prevent stress cracking resistance.
Embodiment
Embodiment 1
The activeness and quietness halogen-free and flame-retardant polycarbonate material of the present embodiment is made up of the component of following weight：
25kg polycarbonate resin, 0.0125kg fire retardant perfluorobutyl potassium sulfonate, 0.1kg composite antioxidant (being made up of 0.025kg antioxidant 1010s and 0.075kg irgasfos 168s), 1kg reinforcing agent is (with crosslink propylene acid esters or organic Silicon is core, and grafted methacrylic acid methyl esters is the compound of shell, and MIT's trade mark is S2001.)
The preparation method of above-mentioned activeness and quietness halogen-free and flame-retardant polycarbonate material has steps of：
(1) polycarbonate resin through drying process, fire retardant, composite antioxidant and toughener will be weighed according to formula to fall Enter mixer high speed and mix 5~6min, discharging, obtain mixed material；
(2) mixed material obtained by step (1) is sent to melting extrusion in double screw extruder, while in extruder machine Exhaust outlet adds 2 strands of alkali-free long glass fibres (equivalent to the addition long glass fibers of 4.5kg alkali-frees in said mixture in the middle part of body Dimension), the billot die head pelletizing extruded and water cooling, activeness and quietness halogen-free and flame-retardant polycarbonate material is produced by drying process Material.
In above-mentioned steps (2), the temperature in each area of double screw extruder is：T1=140 DEG C, T2=230 DEG C, T3=260 DEG C, T4=265 DEG C, T5=275 DEG C, T6=285 DEG C, T7=280 DEG C, T8=275 DEG C, T9=255 DEG C, TMould=255 DEG C.
2~embodiment of embodiment 6
The preparation method of the activeness and quietness halogen-free and flame-retardant polycarbonate material of each embodiment is same as Example 1, difference The weight proportion in each component is in, is specifically shown in Table 1.
Table 1：The prescription of embodiment 1~6 matches
By activeness and quietness halogen-free and flame-retardant polycarbonate material made from 1~embodiment of embodiment 6, noted using injection moulding machine Standard specimen is moulded, and power performance test is carried out to the standard specimen by national standard, test result is shown in Table 2.
Table 2：Activeness and quietness halogen-free and flame-retardant polycarbonate testing of materials result is made in the prescription of embodiment 1~6
Comparative example
The preparation method of the activeness and quietness halogen-free and flame-retardant polycarbonate material of comparative example is identical with embodiment 3 and embodiment 6, Difference is different in component proportion, and the halogen-free and flame-retardant polycarbonate for being not added with reinforcing agent and toughener is contrasted, is specifically shown in Table 3。
Table 3：Embodiment 3, embodiment 6, comparative example prescription proportioning
Embodiment 3 Embodiment 6 Comparative example
Polycarbonate resin 25kg 25kg 25kg
Fire retardant 0.0125kg 0.0125kg 0.0125kg
Toughener 2kg 1.5kg 0
Reinforcing agent 4.5kg 5.5kg 0
Antioxidant 1010 0.025kg 0.025kg 0.025kg
Irgasfos 168 0.075kg 0.075kg 0.075kg
By comparative example halogen-free and flame-retardant polycarbonate using injection moulding machine injection standard specimen, the performance of test, it is specifically shown in Table 4.
Table 4：Activeness and quietness halogen-free and flame-retardant polycarbonate testing of materials knot is made in embodiment 3, embodiment 5, comparative example prescription Fruit
From table 4, the present invention use alkali-free long glass fibres be reinforcing agent and using crosslink propylene acid esters or organosilicon as Core, grafted methacrylic acid methyl esters are that the compound of shell is activeness and quietness halogen-free and flame-retardant polycarbonate and Halogen that toughener obtains Fire-retardant polycarbonate is compared, and comprehensive mechanical property, the heat distortion temperature of halogen-free and flame-retardant polycarbonate can be effectively improved, to fire-retardant effect Fruit influences little.

Claims (9)

1. a kind of activeness and quietness halogen-free and flame-retardant polycarbonate material, it is characterised in that the material is by following components in parts by weight group Into：100 parts, fire retardant 0.04-0.15 of polycarbonate resin, composite antioxidant 0.1-0.4 parts, reinforcing agent 5-30 parts, toughener 2-8 parts.
2. makrolon material according to claim 1, it is characterised in that material is made up of following components in parts by weight：It is poly- 100 parts of carbonate resin, fire retardant 0.05,0.4 part of composite antioxidant, 18 parts of reinforcing agent, 6 parts of toughener.
3. makrolon material according to claim 1, it is characterised in that material is made up of following components in parts by weight：It is poly- 100 parts of carbonate resin, fire retardant 0.05,0.4 part of composite antioxidant, 22 parts of reinforcing agent, 6 parts of toughener.
4. according to the makrolon material described in claim any one of 1-3, it is characterised in that the polycarbonate resin is double Middle viscosity or the high viscosity makrolon of phenol A classes；Described fire retardant is perfluorobutyl potassium sulfonate；Described composite antioxidant by Antioxidant 1010 and irgasfos 168 composition；Described reinforcing agent is alkali-free long glass fibres.
5. makrolon material according to claim 4, it is characterised in that described composite antioxidant is by antioxidant 1010 With irgasfos 168 according to 1: 3 weight than forming.
6. makrolon material according to claim 4, it is characterised in that described toughener is with crosslink propylene acid esters Or organosilicon is core, grafted methacrylic acid methyl esters is the compound of shell.
7. the preparation method of makrolon material according to claim 6, it is characterised in that this method includes following step Suddenly：
(1) by according to formula weigh the polycarbonate resin through drying process, fire retardant, composite antioxidant and toughener pour into it is mixed Conjunction machine high speed mixes 5~6min, discharging, obtains mixed material；
(2) mixed material obtained by step (1) is sent to melting extrusion in double screw extruder, each area of double screw extruder Temperature is：T1=135~145 DEG C, T2=225~235 DEG C, T3=255~265 DEG C, T4=260~270 DEG C, T5=270~280 DEG C, T6=280~290 DEG C, T7=275~285 DEG C, T8=260~270 DEG C, T9=250~260 DEG C, TMould=250~260 DEG C, Long glass fibres, the billot die head pelletizing extruded and water cooling are added in extruder waist exhaust outlet simultaneously, by dry Dry handle produces activeness and quietness halogen-free and flame-retardant polycarbonate material.
8. the preparation method of makrolon material according to claim 7, it is characterised in that in step (2), twin-screw squeezes The temperature in Chu Jige areas is：T1=140 DEG C, T2=230 DEG C, T3=260 DEG C, T4=265 DEG C, T5=275 DEG C, T6=285 DEG C, T7 =280 DEG C, T8=275 DEG C, T9=255 DEG C, TMould=255 DEG C.
9. the preparation method of makrolon material according to claim 8, it is characterised in that step (1) will be according to formula Weigh the polycarbonate resin through drying process, fire retardant, composite antioxidant and toughener and pour into the mixing of mixer high speed 6min。
CN201710999295.1A 2017-10-24 2017-10-24 A kind of activeness and quietness halogen-free and flame-retardant polycarbonate material and preparation method thereof Pending CN107880510A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112538250A (en) * 2020-12-02 2021-03-23 赵光明 Antioxidant plastic formula
US20220064438A1 (en) * 2020-08-27 2022-03-03 Lotte Chemical Corporation Thermoplastic Resin Composition and Article Produced Therefrom

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1810862A (en) * 2006-02-23 2006-08-02 广州金发科技股份有限公司 Continuous long fiber reinforced fire-retardant thermoplastic resin and its prepn
US20080290330A1 (en) * 2007-05-25 2008-11-27 Mitac Precision Technology (Shunde) Ltd. Composition of high impact glass firber reinforced flame-retardant engineering plastic and preparation method thereof
CN104031374A (en) * 2014-06-10 2014-09-10 惠州市沃特新材料有限公司 Polycarbonate composition and preparation method thereof
CN104497532A (en) * 2014-12-17 2015-04-08 安徽科聚新材料有限公司 Halogen-free flame-retardant high-gloss high-glass fiber reinforced PC material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1810862A (en) * 2006-02-23 2006-08-02 广州金发科技股份有限公司 Continuous long fiber reinforced fire-retardant thermoplastic resin and its prepn
US20080290330A1 (en) * 2007-05-25 2008-11-27 Mitac Precision Technology (Shunde) Ltd. Composition of high impact glass firber reinforced flame-retardant engineering plastic and preparation method thereof
CN104031374A (en) * 2014-06-10 2014-09-10 惠州市沃特新材料有限公司 Polycarbonate composition and preparation method thereof
CN104497532A (en) * 2014-12-17 2015-04-08 安徽科聚新材料有限公司 Halogen-free flame-retardant high-gloss high-glass fiber reinforced PC material and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20220064438A1 (en) * 2020-08-27 2022-03-03 Lotte Chemical Corporation Thermoplastic Resin Composition and Article Produced Therefrom
US11781010B2 (en) * 2020-08-27 2023-10-10 Lotte Chemical Corporation Thermoplastic resin composition and article produced therefrom
CN112538250A (en) * 2020-12-02 2021-03-23 赵光明 Antioxidant plastic formula

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