CN103275465A - Preparation method for halogen-free flame-retardant polybutylene terephthalate alloy composite material - Google Patents
Preparation method for halogen-free flame-retardant polybutylene terephthalate alloy composite material Download PDFInfo
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- CN103275465A CN103275465A CN2013101706101A CN201310170610A CN103275465A CN 103275465 A CN103275465 A CN 103275465A CN 2013101706101 A CN2013101706101 A CN 2013101706101A CN 201310170610 A CN201310170610 A CN 201310170610A CN 103275465 A CN103275465 A CN 103275465A
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- polybutylene terephthalate
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- alloy composite
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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
- B29C48/022—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the choice of material
-
- 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
- B29C48/92—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
- B29C2948/92704—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
- B29C2948/9298—Start-up, shut-down or parameter setting phase; Emergency shut-down; Material change; Test or laboratory equipment or studies
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a preparation method for a halogen-free flame-retardant polybutylene terephthalate alloy composite material, which belongs to the technical field of preparation of high polymer materials. The preparation method comprises the following steps of: drying 53-64 parts of polybutylene terephthalate and 9-16 parts of polyamide 6 resin for 12 hours at 110 DEG C; then mixing the dried material, 10-17 parts of olefin resin, 7-11 parts of a compatilizer, 19-27 parts of phosphate, 0.6-1.3 parts of an antioxidant, 10-19 parts of reinforced fibres, and 0.8-1.4 parts of carbon black in a high-speed mixing machine; then transferring the mixture into a parallel double-screw extruder for melt extrusion, and controlling the screw temperatures of the double-screw extruders to be 220-270 DEG C; and discharging from the double-screw extruders, packaging after cooling and slicing, so as to obtain the finished product. The material has the following performance indexes: a tensile strength of 122-141 MPa, a bending strength of 212-226 MPa, a bending modulus of 9000-11000 MPa, a notch impact strength of 62-75 j/m, a thermal deformation temperature of 215-236 DEG C, flame resistance of V-0 (UL-94-1.5 mm); and the material is halogen-free and good in environmental friendliness property.
Description
Technical field
The invention belongs to field of polymer material preparing technology, be specifically related to a kind of preparation method of polybutylene terephthalate alloy composite materials of halogen-free flameproof.
Background technology
Polybutylene terephthalate is a kind of engineering plastic materials that is widely used in fields such as automobile, building, electronic instrument.Along with fire takes place frequently, people deeply are familiar with fire retardant material, think that material itself is fire-retardant to strive for the rescue time for the prevention propagation of flame, and it is very important to save lives and properties.Therefore, most of material all requires the fire-retardant requirement that reaches certain, yet, in order to reach fire-retardant requirement, generally in material, add halogen flame, reach fire-retardant purpose as using halogen containing flame-retardant among the Chinese patent publication number CN1060189A and containing the antimony fire retardant, these fire retardants can produce a large amount of poisonous and harmful smog when burning, and after goods abandon, cause antimony diffusion to water body easily, therefore influence environment for human survival, be necessary with rational preparation method and be aided with the polybutylene terephthalate alloy composite materials that these shortcomings are eliminated in rational material preparation.
Summary of the invention
Task of the present invention is to provide a kind of preparation method of polybutylene terephthalate alloy composite materials of halogen-free flameproof, the polybutylene terephthalate alloy composite materials that is obtained by this method had both helped to ensure desirable intensity and toughness, was conducive to ensure close friend and flame retardant effect excellence to environment again.
Task of the present invention is finished like this, a kind of preparation method of polybutylene terephthalate alloy composite materials of halogen-free flameproof, it is 53～64 parts of polybutylene terephthalates and 9～16 parts of dry 12h under 110 ℃ of polyamide 6 resin that will take by weighing by weight earlier, obtain dried feed, the olefin resin that this dried feed companion is taken by weighing by weight is 10～17 parts again, 7 ~ 11 parts of compatilizers, 19 ~ 27 parts of phosphoric acid salt, 0.6 ~ 1.3 part in oxidation inhibitor, mix 11min in 10 ~ 19 parts of fortifying fibres and 0.8 ~ 1.4 part of input high-speed mixer of carbon black, obtain compound, then compound is changed in the parallel twin screw extruder and melt extrude, the extruder temperature of twin screw extruder is controlled to be 220-270 ℃, go out twin screw extruder and after cooling and pelletizing, pack, obtain the polybutylene terephthalate alloy composite materials of halogen-free flameproof.
In one embodiment of the invention, described polybutylene terephthalate resin is fusing point at 230 ℃ polybutylene terephthalate.
In another embodiment of the present invention, described polyamide 6 resin is fusing point at 220 ℃ polycaprolactam polyimide resin.
In yet another embodiment of the present invention, described olefin resin is the polyvinyl resin of 130 ℃ of fusing points.
In another embodiment of the present invention, described compatilizer is the polyvinyl resin of maleic anhydride graft.
Also have among the embodiment of the present invention, described phosphoric acid salt is hypo-aluminum orthophosphate.
More of the present invention and among embodiment, described oxidation inhibitor is β (3,5-di-t-butyl-4-hydroxybenzene) propionic acid octadecanol ester.
In of the present invention and then embodiment, described fortifying fibre is the alkali free glass fibre of length 6mm.
Of the present invention again more and among embodiment, described carbon black is the carbon black that channel process is produced.
The polybutylene terephthalate alloy composite materials of the halogen-free flameproof that preparation method of the present invention obtains has following performance index after tested: tensile strength 122～141MPa, flexural strength 212～226MPa, modulus in flexure 9000～11000MPa, notched Izod impact strength 62～75j/m, 215～236 ℃ of heat-drawn wires, flame retardant resistance V-0 (UL-94-1.5mm); Material does not contain halogen, has favorable environment protection.
Embodiment
Embodiment 1:
Earlier the fusing point that will take by weighing by weight at 230 ℃ 64 parts of polybutylene terephthalates and fusing point at 9 parts of input drying installations of polycaprolactam polyimide resin of 220 ℃ at 110 ℃ of dry 12h down, obtain dried feed, again with this dried feed in company with the fusing point that takes by weighing by weight 13 parts of 130 ℃ polyvinyl resins, by 7 parts of the polyvinyl resins of maleic anhydride graft, 27 parts of hypo-aluminum orthophosphates, β (3,5-di-t-butyl-4-hydroxybenzene) propionic acid octadecanol ester is 1 part, length is to mix 11min in 15 parts of the alkali free glass fibres of 6mm and 1.4 parts of input high-speed mixers of carbon black of being produced by channel process, obtain compound, then compound is changed in the parallel twin screw extruder and melt extrude, the extruder temperature of twin screw extruder is controlled to be 270 ℃, after going out twin screw extruder, through cooling and pelletizing, pack, obtain the polybutylene terephthalate alloy composite materials of halogen-free flameproof.
Embodiment 2:
Earlier the fusing point that will take by weighing by weight at 230 ℃ 53 parts of polybutylene terephthalates and fusing point at 11 parts of input drying installations of polycaprolactam polyimide resin of 220 ℃ at 110 ℃ of dry 12h down, obtain dried feed, again with this dried feed in company with the fusing point that takes by weighing by weight 17 parts of 130 ℃ polyvinyl resins, by 11 parts of the polyvinyl resins of maleic anhydride graft, 25 parts of hypo-aluminum orthophosphates, β (3,5-di-t-butyl-4-hydroxybenzene) propionic acid octadecanol ester is 1.3 parts, length is to mix 11min in 19 parts of the alkali free glass fibres of 6mm and 0.8 part of input high-speed mixer of carbon black of being produced by channel process, obtain compound, then compound is changed in the parallel twin screw extruder and melt extrude, the extruder temperature of twin screw extruder is controlled to be 220 ℃, after going out twin screw extruder, through cooling and pelletizing, pack, obtain the polybutylene terephthalate alloy composite materials of halogen-free flameproof.
Embodiment 3:
Earlier the fusing point that will take by weighing by weight at 230 ℃ 60 parts of polybutylene terephthalates and fusing point at 16 parts of input drying installations of polycaprolactam polyimide resin of 220 ℃ at 110 ℃ of dry 12h down, obtain dried feed, again with this dried feed in company with the fusing point that takes by weighing by weight 12 parts of 130 ℃ polyvinyl resins, by 9 parts of the polyvinyl resins of maleic anhydride graft, 19 parts of hypo-aluminum orthophosphates, β (3,5-di-t-butyl-4-hydroxybenzene) propionic acid octadecanol ester is 0.6 part, length is to mix 11min in 10 parts of the alkali free glass fibres of 6mm and 1 part of input high-speed mixer of carbon black of being produced by channel process, obtain compound, then compound is changed in the parallel twin screw extruder and melt extrude, the extruder temperature of twin screw extruder is controlled to be 260 ℃, after going out twin screw extruder, through cooling and pelletizing, pack, obtain the polybutylene terephthalate alloy composite materials of halogen-free flameproof.
Embodiment 4:
Earlier the fusing point that will take by weighing by weight at 230 ℃ 57 parts of polybutylene terephthalates and fusing point at 14 parts of input drying installations of polycaprolactam polyimide resin of 220 ℃ at 110 ℃ of dry 12h down, obtain dried feed, again with this dried feed in company with the fusing point that takes by weighing by weight 15 parts of 130 ℃ polyvinyl resins, by 8 parts of the polyvinyl resins of maleic anhydride graft, 24 parts of hypo-aluminum orthophosphates, β (3,5-di-t-butyl-4-hydroxybenzene) propionic acid octadecanol ester is 0.9 part, length is to mix 11min in 16 parts of the alkali free glass fibres of 6mm and 1.2 parts of input high-speed mixers of carbon black of being produced by channel process, obtain compound, then compound is changed in the parallel twin screw extruder and melt extrude, the extruder temperature of twin screw extruder is controlled to be 245 ℃, after going out twin screw extruder, through cooling and pelletizing, pack, obtain the polybutylene terephthalate alloy composite materials of halogen-free flameproof.
The polybutylene terephthalate alloy composite materials of the halogen-free flameproof that is obtained by above-described embodiment 1 to 4 has following technique effect after tested:
| Test event | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Tensile strength MPa | 122 | 128 | 134 | 140 |
| Flexural strength MPa | 213 | 216 | 221 | 226 |
| Modulus in flexure MPa | 9070 | 9780 | 10350 | 10980 |
| Notched Izod impact strength j/m | 62.4 | 67.7 | 71.4 | 74.4 |
| Heat-drawn wire ℃ | 216 | 222 | 228 | 235 |
| Flame retardant resistance (UL-94-V-0-1.5mm) | V-0 | V-0 | V-0 | V-0 |
Claims (9)
1.
A kind of preparation method of polybutylene terephthalate alloy composite materials of halogen-free flameproof, it is characterized in that it is 53～64 parts of polybutylene terephthalates and 9～16 parts of dry 12h under 110 ℃ of polyamide 6 resin that will take by weighing by weight earlier, obtain dried feed, the olefin resin that this dried feed companion is taken by weighing by weight is 10～17 parts again, 7 ~ 11 parts of compatilizers, 19 ~ 27 parts of phosphoric acid salt, 0.6 ~ 1.3 part in oxidation inhibitor, mix 11min in 10 ~ 19 parts of fortifying fibres and 0.8 ~ 1.4 part of input high-speed mixer of carbon black, obtain compound, then compound is changed in the parallel twin screw extruder and melt extrude, the extruder temperature of twin screw extruder is controlled to be 220-270 ℃, go out twin screw extruder and after cooling and pelletizing, pack, obtain the polybutylene terephthalate alloy composite materials of halogen-free flameproof.
2.
The preparation method of the polybutylene terephthalate alloy composite materials of halogen-free flameproof according to claim 1 is characterized in that described polybutylene terephthalate resin is fusing point at 230 ℃ polybutylene terephthalate.
3.
The preparation method of the polybutylene terephthalate alloy composite materials of halogen-free flameproof according to claim 1 is characterized in that described polyamide 6 resin is fusing point at 220 ℃ polycaprolactam polyimide resin.
4.
The preparation method of the polybutylene terephthalate alloy composite materials of halogen-free flameproof according to claim 1 is characterized in that described olefin resin is the polyvinyl resin of 130 ℃ of fusing points.
5.
The preparation method of the polybutylene terephthalate alloy composite materials of halogen-free flameproof according to claim 1 is characterized in that described compatilizer is the polyvinyl resin of maleic anhydride graft.
6.
The preparation method of the polybutylene terephthalate alloy composite materials of halogen-free flameproof according to claim 1 is characterized in that described phosphoric acid salt is hypo-aluminum orthophosphate.
7.
The preparation method of the polybutylene terephthalate alloy composite materials of halogen-free flameproof according to claim 1 is characterized in that described oxidation inhibitor is β (3,5-di-t-butyl-4-hydroxybenzene) propionic acid octadecanol ester.
8.
The preparation method of the polybutylene terephthalate alloy composite materials of halogen-free flameproof according to claim 1 is characterized in that described fortifying fibre is the alkali free glass fibre of length 6mm.
9.
The preparation method of the polybutylene terephthalate alloy composite materials of halogen-free flameproof according to claim 1 is characterized in that described carbon black is the carbon black that channel process is produced
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101706101A CN103275465A (en) | 2013-05-10 | 2013-05-10 | Preparation method for halogen-free flame-retardant polybutylene terephthalate alloy composite material |
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| CN2013101706101A CN103275465A (en) | 2013-05-10 | 2013-05-10 | Preparation method for halogen-free flame-retardant polybutylene terephthalate alloy composite material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104599776A (en) * | 2014-12-31 | 2015-05-06 | 东莞市高能磁电技术有限公司 | Halogen-free flame-retardant insulated electric cable using polybutylene terephthalate composite material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102918108A (en) * | 2010-05-27 | 2013-02-06 | 胜技高分子株式会社 | Polybutylene terephthalate resin composition |
| CN103013060A (en) * | 2012-11-28 | 2013-04-03 | 宁波长阳科技有限公司 | Polyethylene toughening thermoplastic polyester composite material and preparation method thereof |
-
2013
- 2013-05-10 CN CN2013101706101A patent/CN103275465A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102918108A (en) * | 2010-05-27 | 2013-02-06 | 胜技高分子株式会社 | Polybutylene terephthalate resin composition |
| CN103013060A (en) * | 2012-11-28 | 2013-04-03 | 宁波长阳科技有限公司 | Polyethylene toughening thermoplastic polyester composite material and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104599776A (en) * | 2014-12-31 | 2015-05-06 | 东莞市高能磁电技术有限公司 | Halogen-free flame-retardant insulated electric cable using polybutylene terephthalate composite material |
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Application publication date: 20130904 |