CN105542305A - Halogen-free high-temperature-resisting flame-resistant material high in oxygen index and preparation method and application thereof - Google Patents
Halogen-free high-temperature-resisting flame-resistant material high in oxygen index and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to halogen-free high-temperature-resisting flame-resistant material high in oxygen index and a preparation method and application thereof. The halogen-free high-temperature-resisting flame-resistant material is prepared from, by weight, 100 parts of carrier resin, 200-400 parts of a flame retardant, 5-12 parts of a synergistic effect additive, 2-6 parts of a surface active agent and 0.2-3 parts of an antioxidant. The flame retardant is first fully treated by using the surface active agent and then is fully and evenly mixed with the synergistic effect additive and the antioxidant, the mixture is added into a double-screw extruder to be extruded out and palletized, the obtained halogen-free high-temperature flame-resistant masterbatch and the carrier resin are subjected to LFT-D online extrusion molding to obtain the high-oxygen-index halogen-free high-temperature flame-resistant masterbatch. Compared with the prior art, the product prepared by means of the preparation method has very high oxygen index, excellent flame retardancy, processability and mechanical properties and meanwhile is low in processing cost, industrialization is easy to achieve, the preparation method can be combined with an LFT-D online molding technology, and the application prospect is very wide.
Description
Technical field
The present invention relates to technical field of polymer materials, especially relate to halogen-free refractory fire retardant material of a kind of high oxygen index and its preparation method and application.
Background technology
Public place security against fire is concerning the life of people, if some communal facility non-flame-retardant material are made, once presence of fire, consequence is hardly imaginable.Our country is to the material of some equipment, and the bottom PLASTIC LAMINATED etc. as the finishing material in the public chair of stadiums, EMUs car and motor car engine requires more and more stricter, all makes strict rules the oxygen index of material, flame retardant resistance and smoke density.
Fire retardant the most frequently used is at present that eight bromo ether, decabromodiphenyl oxide etc. are containing brominated flame retardant, this based flame retardant has good flame retardant resistance, but a large amount of hazardous and noxious substances can be produced during brominated material combustion, the skin of grievous injury human body and liver, cause human body deformity and have carcinogenesis, other halogen flame retardant materials also can discharge hazardous and noxious substances when burning.The key addressed this problem, is the selection of fire retardant material.
Chinese patent CN105061854A discloses a kind of halogen-free anti-flaming polyolefin material and uses thereof, by polyolefine 15-50%, inorganic combustion inhibitor 45-80%, organic nano additive 0.1-5%, auxiliary agent 0.1-5% forms, product has high flame retardant, low cigarette, nontoxic advantage, can be widely used as the interior material of fireproof aluminum-plastic board core, fire-resistant cable material, high ferro.Although the method can obtain the good flame retardant polyolefine material of flame retardant resistance, because the addition of inorganics is large, causes the mechanical property of material to decline more, particularly show the loss on the workability of material, intensity and limiting oxygen index(LOI).
Summary of the invention
Object of the present invention is exactly the defect existed to overcome above-mentioned prior art, and provides halogen-free refractory flame-retardant master batch of a kind of high oxygen index, excellent flame retardancy, processibility and mechanical property and its preparation method and application.
Object of the present invention can be achieved through the following technical solutions:
A halogen-free refractory flame-retardant master batch for high oxygen index, adopts the raw material of following component and weight part content:
Vector resin 100, fire retardant 200-400, synergistic auxiliary agent 5-12, tensio-active agent 2-6, oxidation inhibitor 0.2-3.
Described vector resin is the polypropylene of melt mass flow rate 40-100g/10min.
Described fire retardant is selected from one or both mixtures of melamine cyanurate, melamine polyphosphate or ammonium polyphosphate.
Described synergistic auxiliary agent be selected from maleic anhydride, dimethyl diphenyl hexane, dimethyldiphenylbutane, poly-diisopropyl benzene, calcium stearate, polyethylene wax or silicone oil one or more, as preferred embodiment, synergistic auxiliary agent adopts dimethyl diphenyl hexane, dimethyldiphenylbutane or poly-diisopropyl benzene.
Described tensio-active agent be selected from molecular weight be 1000 ~ 20000 γ-aminopropyl triethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane or sec.-propyl three different titanium acyl titanic acid ester one or both mixtures, as preferred embodiment, tensio-active agent employing molecular weight is γ-glycidyl ether oxygen propyl trimethoxy silicane or the γ-methacryloxypropyl trimethoxy silane of 5000 ~ 10000.
Described oxidation inhibitor is selected from four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, tricresyl phosphite (2,4-di-tert-butyl) ester, the two octadecyl ester of thio-2 acid, the two lauryl or 1 of thio-2 acid, 3, one or both mixtures of 5-tri-(3,5-di-tert-butyl-4-hydroxyl benzyl) tricarbimide.
The preparation method of halogen-free refractory flame-retardant master batch, adopts following steps:
(1) after getting the raw materials ready by formula, first tensio-active agent is mixed with fire retardant in high-speed mixer, utilize tensio-active agent fully to process fire retardant, more fully mix with vector resin, synergistic auxiliary agent, oxidation inhibitor;
(2) be added in twin screw extruder by said mixture, the screw slenderness ratio controlling twin screw extruder is 40-46, and twin screw extruder each district temperature range is 160-220 DEG C, extrudes pelletizing, namely obtains the halogen-free refractory flame-retardant master batch of high oxygen index.
The mode of pelletizing is selected from the one of water-cooled pelletizing, air-cooled flour milling pelletizing or the pelletizing of water ring flour milling, and as preferred embodiment, the mode of pelletizing adopts air-cooled flour milling pelletizing.
The application of the halogen-free refractory flame-retardant master batch of high oxygen index, by the polypropylene of halogen-free refractory flame-retardant master batch and melt mass flow rate 40-100g/10min in mass ratio for 30-50:100 mixes, then mold pressing is extruded online through LFT-D, the content of the online moulding press continuous fibre of control LFT-D is at 20wt%, selected continuous glass fibre is adopt filament diameter to be the special continuous glass fibre of the online mold pressing of LFT-D of 17 microns, obtains the halogen-free refractory fire retardant material of high oxygen index.
Compared with prior art, halogen-free refractory flame-retardant master batch prepared by the present invention, owing to have employed the vector resin of melt mass flow rate 40-100g/10min, in addition, tensio-active agent is selected from the γ-aminopropyl triethoxysilane that molecular weight is 1000 ~ 20000, γ-glycidyl ether oxygen propyl trimethoxy silicane, one or both mixtures of γ-methacryloxypropyl trimethoxy silane or sec.-propyl three different titanium acyl titanic acid ester, through the well-mixed fire retardant of tensio-active agent in processibility, temperature tolerance and limiting oxygen index(LOI) there is lifting by a relatively large margin, when molecular weight is less than 1000, time, because molecular weight is too small, effective activity can not be formed with the surface of fire retardant, fire retardant covered effect is poor), when molecular weight is greater than 20000, because molecular weight is excessive, the coated difficulty of fire retardant is large, processibility can be caused to reduce simultaneously, make the product surface outward appearance prepared, limiting oxygen index(LOI), mechanical property all cannot obtain good effect.
In addition, the present invention can combine with the online mould pressing technology of LFT-D, because the flow rate that have employed preferred vector resin is 40-100g/10min, the selection of tensio-active agent middle-molecular-weihydroxyethyl, these the apparatus processing performance preferably combining LFT-D completely, with the combination of continuous glass fibre, the loss of end properties can not be caused.And due to inorganics used in the present invention considerably less, therefore the limiting oxygen index(LOI) of material and mechanical property can fully maintain.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
A preparation method for the halogen-free refractory flame-retardant master batch of high oxygen index, adopts following steps:
Get the raw materials ready according to following component and weight part: polypropylene 100, fire retardant 350, synergistic auxiliary agent 6, tensio-active agent 4, oxidation inhibitor 1, the polyacrylic MFR wherein used is 40g/10min, fire retardant is the mixture of melamine cyanurate and melamine polyphosphate, synergistic auxiliary agent is maleic anhydride, tensio-active agent is molecular weight is the γ-aminopropyl triethoxysilane of 1000 and the mixture of γ-glycidyl ether oxygen propyl trimethoxy silicane, oxidation inhibitor is four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester.
First fire retardant is fully processed through tensio-active agent, masterbatch is prepared through being mixed to join in parallel dual-screw extruding machine to extrude again with remaining component, the screw slenderness ratio of twin screw extruder is 40, temperature each district setting of twin screw extruder is respectively: 160 DEG C-175 DEG C-180 DEG C-185 DEG C-195 DEG C-210 DEG C-210 DEG C-210 DEG C-220 DEG C-220 DEG C-220 DEG C, then carry out a point cold grinding face pelletizing, namely obtain halogen-free refractory flame-retardant master batch.
Again halogen-free refractory flame-retardant master batch is mixed with polypropylene, mold pressing is extruded through German Dieffenbacher LFT-D mould pressing production line, after mold pressing, in goods, the content of continuous fibre controls at 20wt%, prepared goods are cut into the test bars test for subsequent use of required specification, batten specification: the wide 30mm of long 80mm-, long 80mm-10mm, the wide 13mm of long 125mm-, thickness are all 4.28mm, test flame retardant properties, mechanical property, limiting oxygen index(LOI).
Embodiment 2
A preparation method for the halogen-free refractory flame-retardant master batch of high oxygen index, adopts following steps:
Get the raw materials ready according to following component and weight: polypropylene 100, fire retardant 330, synergistic auxiliary agent 8, tensio-active agent 3, oxidation inhibitor 2.The polyacrylic MFR wherein used is 60g/10min, fire retardant is ammonium polyphosphate, synergistic auxiliary agent is the mixture of calcium stearate and polyethylene wax, tensio-active agent to be molecular weight be 2000 sec.-propyl three different titanium acyl titanic acid ester, oxidation inhibitor is 1,3,5-tri-(3,5-di-tert-butyl-4-hydroxyl benzyl) tricarbimide.
First fire retardant is fully processed through tensio-active agent, masterbatch is prepared through being mixed to join in parallel dual-screw extruding machine to extrude again with remaining component, the screw slenderness ratio of twin screw extruder is 44, temperature each district setting of twin screw extruder is respectively: 160 DEG C-175 DEG C-180 DEG C-185 DEG C-195 DEG C-210 DEG C-210 DEG C-210 DEG C-220 DEG C-220 DEG C-220 DEG C, then carry out a point cold grinding face pelletizing, namely obtain halogen-free refractory flame-retardant master batch.
Again halogen-free refractory flame-retardant master batch is mixed with polypropylene, mold pressing is extruded through German Dieffenbacher LFT-D mould pressing production line, after mold pressing, in goods, the content of continuous fibre controls at 20wt%, prepared goods are cut into the test bars test for subsequent use of required specification, batten specification: the wide 30mm of long 80mm-, long 80mm-10mm, the wide 13mm of long 125mm-, thickness are all 4.28mm, test flame retardant properties, mechanical property, limiting oxygen index(LOI).
Comparative example 1
Adopt the proportioning of a brominated fire retardant material general at present: PP resin 480, PP-g-MAH30, TDE 200, weisspiessglanz 100, EBS5, antioxidant 1010 3, DLTDP2.5.
First above-mentioned all material is mixed through mixing machine according to proportioning, join extruding pelletization in parallel dual-screw extruding machine again, dual-screw-stem machine each district temperature is 170 DEG C-175 DEG C-180 DEG C-185 DEG C-195 DEG C-210 DEG C-210 DEG C-210 DEG C-220 DEG C-220 DEG C-220 DEG C, then to its water cooling rear haulage pelletizing.Again by prepared material after German Dieffenbacher LFT-D mould pressing production line extrudes mold pressing, prepared goods are cut into the test bars test for subsequent use of required specification, batten specification: the wide 30mm of long 80mm-, long 80mm-10mm, the wide 13mm of long 125mm-, thickness are all 4.28mm, test flame retardant properties, mechanical property, limiting oxygen index(LOI).
The product test result of table 1 embodiment and comparative example
Can be found out by Data Comparison in table 1, embodiment all will far away higher than comparative example in flame retardant properties, mechanical property and limiting oxygen index(LOI) performance, meet the standard-required of track traffic (seat) thermoplastics TB/T3237-2010 completely, and comparative example can not meet the demands.Embodiment advantage is fairly obvious, can arrive the requirement of environmental protection, Halogen, high temperature resistant, high oxygen index completely.
Embodiment 3
A preparation method for the halogen-free refractory flame-retardant master batch of high oxygen index, adopts following steps:
Get the raw materials ready according to following component and weight: polypropylene 100, its MFR is 40g/10min, fire retardant is melamine cyanurate 200, synergistic auxiliary agent maleic anhydride 5, tensio-active agent to be molecular weight be 5000 γ-aminopropyl triethoxysilane 2, irgasfos 168 0.2.
First fire retardant is fully processed through tensio-active agent, again with remaining ingredient through being mixed to join in parallel dual-screw extruding machine, the screw slenderness ratio of twin screw extruder is 40, temperature each district setting of twin screw extruder is respectively: 160 DEG C-175 DEG C-180 DEG C-185 DEG C-195 DEG C-210 DEG C-210 DEG C-210 DEG C-220 DEG C-220 DEG C-220 DEG C, then carry out a point cold grinding face pelletizing, namely obtain halogen-free refractory flame-retardant master batch.
The halogen-free refractory flame-retardant master batch obtained and MFR are that the acrylic resin of 40g/10min is in mass ratio for 30:100 mixes, then mold pressing is extruded online through LFT-D, the content of the online moulding press continuous fibre of control LFT-D is at 20wt%, the continuous fibre adopted in the present embodiment to be filament diameter the be special continuous glass fibre of the online mold pressing of LFT-D of 17 microns, prepares the halogen-free refractory fire retardant material of high oxygen index.
Embodiment 4
A preparation method for the halogen-free refractory flame-retardant master batch of high oxygen index, adopts following steps:
Get the raw materials ready according to following component and weight: polypropylene 100, its MFR is 70g/10min, fire retardant is melamine polyphosphate 300, synergistic auxiliary agent is maleic anhydride 8, tensio-active agent to be molecular weight be 10000 γ-aminopropyl triethoxysilane 4, antioxidant 1010 1.6.
First fire retardant is fully processed through tensio-active agent, again with remaining ingredient through being mixed to join in parallel dual-screw extruding machine, the screw slenderness ratio of twin screw extruder is 43, temperature each district setting of twin screw extruder is respectively: 170 DEG C-175 DEG C-180 DEG C-185 DEG C-195 DEG C-210 DEG C-210 DEG C-210 DEG C-220 DEG C-220 DEG C-220 DEG C, then carry out a point cold grinding face pelletizing, namely obtain the halogen-free refractory flame-retardant master batch of oxygen index.
The halogen-free refractory flame-retardant master batch obtained and MFR be the acrylic resin of 50g/10min in mass ratio for 40:100 mixes, then extrude mold pressing online through LFT-D, obtain the halogen-free refractory fire retardant material of high oxygen index.
By the polypropylene of halogen-free refractory flame-retardant master batch and melt mass flow rate 40-100g/10min in mass ratio for 30-50:100 mixes, then mold pressing is extruded online through LFT-D, the content of the online moulding press continuous fibre of control LFT-D is at 20wt%, the continuous fibre adopted in the present embodiment to be filament diameter the be special continuous glass fibre of the online mold pressing of LFT-D of 17 microns, prepares the halogen-free refractory fire retardant material of high oxygen index.
Embodiment 5
A preparation method for the halogen-free refractory flame-retardant master batch of high oxygen index, adopts following steps:
Get the raw materials ready according to following component and weight: polypropylene 100, its MFR is 100g/10min, and fire retardant is ammonium polyphosphate 400, synergistic auxiliary agent dimethyl diphenyl hexane 12, tensio-active agent be molecular weight are the sec.-propyl three different titanium acyl titanic acid ester of 20000 and mixture 6, the antioxidant 1010 3 of γ-glycidyl ether oxygen propyl trimethoxy silicane.
First fire retardant is fully processed through tensio-active agent, again with remaining ingredient through being mixed to join in parallel dual-screw extruding machine, the screw slenderness ratio of twin screw extruder is 46, temperature each district setting of twin screw extruder is respectively: 170 DEG C-175 DEG C-180 DEG C-185 DEG C-195 DEG C-210 DEG C-210 DEG C-210 DEG C-220 DEG C-220 DEG C-220 DEG C, then carry out a point cold grinding face pelletizing, namely obtain halogen-free refractory flame-retardant master batch.
The halogen-free refractory flame-retardant master batch obtained and MFR be the acrylic resin of 100g/10min in mass ratio for 50:100 mixes, then extrude mold pressing online through LFT-D, obtain the halogen-free refractory fire retardant material of high oxygen index.
By the polypropylene of halogen-free refractory flame-retardant master batch and melt mass flow rate 40-100g/10min in mass ratio for 30-50:100 mixes, then mold pressing is extruded online through LFT-D, the content of the online moulding press continuous fibre of control LFT-D is at 20wt%, the continuous fibre adopted in the present embodiment to be filament diameter the be special continuous glass fibre of the online mold pressing of LFT-D of 17 microns, prepares the halogen-free refractory fire retardant material of high oxygen index.
Claims (10)
1. a halogen-free refractory flame-retardant master batch for high oxygen index, is characterized in that, adopts the raw material of following component and weight part content:
Vector resin 100, fire retardant 200-400, synergistic auxiliary agent 5-12, tensio-active agent 2-6, oxidation inhibitor 0.2-3.
2. the halogen-free refractory flame-retardant master batch of a kind of high oxygen index according to claim 1, is characterized in that, described vector resin is the polypropylene of melt mass flow rate 40-100g/10min.
3. the halogen-free refractory flame-retardant master batch of a kind of high oxygen index according to claim 1, is characterized in that, described fire retardant is selected from one or both mixtures of melamine cyanurate, melamine polyphosphate or ammonium polyphosphate.
4. the halogen-free refractory flame-retardant master batch of a kind of high oxygen index according to claim 1, it is characterized in that, described synergistic auxiliary agent be selected from maleic anhydride, dimethyl diphenyl hexane, dimethyldiphenylbutane, poly-diisopropyl benzene, calcium stearate, polyethylene wax or silicone oil one or more, preferably adopt dimethyl diphenyl hexane, dimethyldiphenylbutane or poly-diisopropyl benzene.
5. the halogen-free refractory flame-retardant master batch of a kind of high oxygen index according to claim 1, it is characterized in that, described tensio-active agent be selected from molecular weight be 1000 ~ 20000 γ-aminopropyl triethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane or sec.-propyl three different titanium acyl titanic acid ester one or both mixtures, preferred molecular weight is γ-glycidyl ether oxygen propyl trimethoxy silicane or the γ-methacryloxypropyl trimethoxy silane of 5000 ~ 10000.
6. the halogen-free refractory flame-retardant master batch of a kind of high oxygen index according to claim 1, it is characterized in that, described oxidation inhibitor is selected from four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, tricresyl phosphite (2,4-di-tert-butyl) ester, the two octadecyl ester of thio-2 acid, the two lauryl or 1 of thio-2 acid, one or both mixtures of 3,5-tri-(3,5-di-tert-butyl-4-hydroxyl benzyl) tricarbimide.
7. the preparation method of the halogen-free refractory flame-retardant master batch of high oxygen index as claimed in claim 1, is characterized in that, the method adopts following steps:
(1) after getting the raw materials ready by formula, first tensio-active agent is mixed with fire retardant in high-speed mixer, more fully mix with vector resin, synergistic auxiliary agent, oxidation inhibitor;
(2) be added in twin screw extruder by said mixture, the screw slenderness ratio controlling twin screw extruder is 40-46, and twin screw extruder each district temperature range is 160-220 DEG C, extrudes pelletizing, namely obtains the halogen-free refractory flame-retardant master batch of high oxygen index.
8. the preparation method of the halogen-free refractory flame-retardant master batch of a kind of high oxygen index according to claim 7, is characterized in that, the mode of pelletizing is selected from the one of water-cooled pelletizing, air-cooled flour milling pelletizing or the pelletizing of water ring flour milling, is preferably air-cooled flour milling pelletizing.
9. the application of the halogen-free refractory flame-retardant master batch of a kind of high oxygen index as claimed in claim 1, it is characterized in that, by the polypropylene of halogen-free refractory flame-retardant master batch and melt mass flow rate 40-100g/10min in mass ratio for 30-50:100 mixes, then mold pressing is extruded online through LFT-D, the content of the online moulding press continuous fibre of control LFT-D, at 20wt%, obtains the halogen-free refractory fire retardant material of high oxygen index.
10. the preparation method of the halogen-free refractory flame-retardant master batch of a kind of high oxygen index according to claim 9, is characterized in that, described continuous fibre to be filament diameter the be special continuous glass fibre of the online mold pressing of LFT-D of 17 microns.
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| CN102558850A (en) * | 2011-12-13 | 2012-07-11 | 中国科学院宁波材料技术与工程研究所 | Flame-retardant functional masterbatch special for nylon 6 and preparation method for masterbatch |
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