CN101787174B - Low-L value inflaming retarding ABS modified resin and preparation method thereof - Google Patents
Low-L value inflaming retarding ABS modified resin and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a low-L value (less than 27) inflaming retarding ABS modified resin and a preparation method thereof. The resin comprises the components with the content (based on parts by weight): 100 parts of ABS resin, 10-25 parts of brominated flame retardant, 20-40 parts of inorganic inflaming retarding master batch, 0.1-0.5 part of anti-dripping agent, 0.2-1 part of antioxidant, 0.1-0.5 part of light stabilizer, 1-3 parts of lubricating agent and 1-4 parts of black master batch. Compared with the prior art, the invention has reasonable technique, overcomes the defect of high L value (namely, low degree of blackness) of the existing inflaming retarding ABS resin, and adopts the novel high-efficiency inflaming retarding synergistic effect technology. The invention leads the resin has higher degree of blackness by reasonably selecting the grain diameter of antimony trioxide, a carbon black lubricating dispersion system and the processing technique of a master batch method on the basis of maintaining the excellent performance of the inflaming retarding ABS resin, and has wide application prospect in the field of the requirement of high degree of blackness.
Description
Technical field
The present invention relates to technical field of polymer materials, relate in particular to fire retardant modified ABS resin of low-L value and preparation method thereof.
Background technology
Acrylonitrile-butadiene-styrene copolymer resin (ABS), have the excellent comprehensive physical property such as high impact, high heat-resisting and low temperature resistant, resistance to chemical attack, electrical insulation capability, and have good processing characteristics, electroplate performance and high gloss outward appearance, be consumption maximum, purposes one of engineering plastics the most widely, be widely used in the fields such as electronics, Communication Equipment, automotive industry, household electrical appliance, office equipment, electric product.
But the ABS resin oxygen index is only 18.3-20, belongs to inflammable macromolecular material, when being used for having the products such as various electronic apparatuss of fire-retardant requirement, need to carry out flame-retardant modified, to satisfy the service requirements of fire safety.
At present, the flame-retardant system that ABS is commonly used is halogenated flame retardant and antimonous oxide synergistic system, and these flame-retardant systems are given flame retardant properties and the comprehensive physical property of ABS excellence.Antimonous oxide is commonly called as " stibium trioxide ", and refractive index reaches 2.1, thereby has very strong opacifying power; And a large amount of interpolations of bromide fire retardant also can affect the background color of flame-proof ABS, so the blackness of flame-proof ABS is usually relatively low, and (the L value is to weigh the index of black, its value is lower, and blackness is higher), require higher panel at blackness, when product uses, just can not reach service requirements.When for example flame-proof ABS replaces black flame-retardant PC/ABS cheaply, tend to because blackness is too low, the too high appearance component that makes of L value does not reach requirement.
At present, the direct effective means of blackness that increases flame-proof ABS is the amount that increases black agglomerate, when but black agglomerate adds certain content to, not obvious to the contribution that the L value reduces, and the adding of a large amount of carbon blacks, can the first mate affect the physicals of flame-proof ABS, increase the risk that flame-proof ABS glows, promote migration and the bloom of wax class dispersion agent in Masterbatch, but also can increase substantially the cost of flame-proof ABS.
Summary of the invention
Purpose of the present invention is exactly to provide fire retardant modified ABS resin of a kind of excellent performance, good flame retardation effect, low-L value (less than 27) and preparation method thereof for the defective that overcomes above-mentioned prior art existence.
Purpose of the present invention can be achieved through the following technical solutions:
A kind of fire retardant modified ABS resin of low-L value is characterized in that, this resin comprises following component and content (weight part):
ABS resinoid 100;
Bromide fire retardant 10-25;
Inorganic fire-retarded master batch 20-40;
Anti-dripping agent 0.1-0.5;
Oxidation inhibitor 0.2-1;
Photostabilizer 0.1-0.5;
Lubricant 1-3;
Black agglomerate 1-4.
Described ABS resinoid is acrylonitrile-butadiene-styrene copolymer (ABS), acrylonitrile-butadiene-acrylate copolymer (ASA), MBS (MBS) or vinyl cyanide-terpolymer EP rubber-styrol copolymer (AES).
Described bromide fire retardant is tetrabromo-bisphenol, TDE, three (bromophenyl) triazine (FR245), brominated epoxy, decabromodiphenyl oxide, hexabromocyclododecane, PHT4, hexabromobenzene, octabromodiphenyl ether, one or several mixtures in Brominated Polystyrene; Described inorganic fire-retarded master batch is take ABS resin as carrier, load Sb system fire retardant 5-30wt% and zinc borate 5-30wt%.
Described Sb system fire retardant is antimonous oxide, a kind of in antimony peroxide or sodium antimonate.
Described anti-dripping agent is that molecular weight is 3,000,000-5,000,000 tetrafluoroethylene (PTFE).
Described oxidation inhibitor is the refine Irganox 1010 of company of CIBA, one or several mixtures of Irganox 1076 or Irganox 168; Described photostabilizer is the 2-dihydroxy benaophenonel, salicylate class, diphenyl phosphite, triphenyl phosphite, one or several mixtures in hydroxybenzotriazole; Described lubricant is silicone oil, white mineral oil, fatty acid amide, barium stearate, Magnesium Stearate, paraffin, polyethylene wax or ethylene bis stearic acid amide, ethylene-vinyl acetate copolymer, one or several mixtures in ethylene-acrylic acid copolymer.
Described black agglomerate is the complex body take polyolefine or ethylene-vinyl acetate copolymer as carrier loaded carbon black, and described content of carbon black is 20-60wt%, and described polyolefinic molecular weight is 2000-10000.
A kind of preparation method of fire retardant modified ABS resin of low-L value is characterized in that, the method comprises the following steps:
(1) get the raw materials ready according to following component and content (weight part):
ABS resinoid 100;
Bromide fire retardant 10-25;
Inorganic fire-retarded master batch 20-40;
Anti-dripping agent 0.1-0.5;
Oxidation inhibitor 0.2-1;
Photostabilizer 0.1-0.5;
Lubricant 1-3;
Black agglomerate 1-4;
(2) use twin screw extruder, take Sb system fire retardant and zinc borate as raw material, the inorganic fire-retarded master batch of preparation take ABS resin as carrier;
(3) the inorganic fire-retarded master batch and the ABS resinoid that step (2) are obtained, after bromide fire retardant, anti-dripping agent, oxidation inhibitor, photostabilizer, lubricant, black agglomerate stir in high-speed mixer and fully mix, send in twin screw extruder through measuring apparatus, the conveying of screw rod, shearing and mixing under, material melting, compound, again through extrude, tie rod, cooling, pelletizing step, obtain the fire retardant modified ABS resin of low-L value.
In described inorganic fire-retarded master batch, the weight content of Sb system fire retardant and zinc borate is 5%-30%.
The screw slenderness ratio of described twin screw extruder is 40, and with temperature control unit and vacuum extractor; The extrusion temperature of described extrusion step is between 190-230 ℃, and screw speed is 100-300 rev/min.
The anti-dripping agent that the present invention selects is the polytetrafluoroethylene PTFE of high molecular, and shell is coated by acrylonitrile styrene resin (AS) (SAN), increases the dispersiveness of PTFE.And itself and the composite use of bromine antimony flame-retardant system have greatly improved flame retarding efficiency, thereby can reduce the consumption of fire retardant, reduce the opacifying power to color.
The present invention selects bromine content high (bromine content is greater than 60%), and on the little bromide fire retardant of physical property impact, thereby the consumption of reduce bromide fire retardant reduces the impact on color, as selects FR245, decabromodiphenyl oxide etc.
It is 2-10 μ m that the present invention selects the particle diameter of Sb system fire retardant, rather than the particle diameter about 1 conventional μ m.Its purpose is to reduce to reduce the specific surface area of Sb system fire retardant, thereby reduces the opacifying power of color.Excessive particle diameter can worsen the fire-retardant and impact property of ABS material.Adopt the zinc borate of 3-8 μ m as fire-retardant compound system, on the one hand, the refractive index of zinc borate is only 1.58, and is less to the opacifying power of color; On the other hand, zinc borate can produce certain fire-retardant synergy with halogenated flame retardant, and flame retarding efficiency is higher.
The present invention adopts the master batch method complete processing of Sb system fire retardant and zinc borate, improves the dispersiveness of Sb system fire retardant and zinc borate, improves flame retarding efficiency.
The present invention selects excellent lubricated composite dispersion system, can effectively promote the dispersion of black agglomerate, strengthens its tinting strength.In the present invention take the Color of polyethylene wax and polarity macromolecule wax compound system as good, as polyethylene wax and ethylene-acrylic acid copolymer compound system, polyethylene wax and ethylene-vinyl acetate copolymer compound system.
The present invention prepares the method for the flame-proof ABS resin of low-L value, adopts twin screw extrusion process equipment, has a technical process simple, and continuously, production efficiency is high, and the characteristics such as constant product quality can be widely used in having the household electrical appliances of higher blackness requirement, the industries such as automobile industry.
In sum, the innovation of the fire retardant modified ABS resin of low-L value of the present invention is:
1. adopt the fire-retardant collaboration system of efficient halogen-antimony-boron-PTFE, the complete processing of master batch method is guaranteeing to have reduced fire retardant on the basis of flame retardant resistance, the consumption of Sb system fire retardant especially, thus reduced its impact on blackness.
2. adopt the Sb system fire retardant of large particle diameter and the compound system of zinc borate, further reduced the impact on the flame-proof ABS blackness.
3. adopt efficient carbon black dispersion lubricating system, greatly increase its tinting strength, thus the fire retardant modified ABS resin of the higher blackness of preparation.
Compared with prior art, technique of the present invention is reasonable, overcome existing flame-proof ABS blackness shortcoming relatively on the low side, adopted the fire-retardant collaboration system of efficient halogen-antimony-boron-PTFE, the particle diameter of choose reasonable antimonous oxide, carbon black lubricates dispersion system, and the complete processing of master batch method, improving on the former premium properties of ABS resin basis, give resin higher blackness, the L value is reached below 27, have broad prospect of application.
Embodiment
The invention will be further described below in conjunction with specific embodiment.
The embodiment preparation method of following master batch method is as follows:
At first use twin screw extruder preparation take ABS as the ratio of the antimonous oxide of carrier and the zinc borate 25% inorganic fire-retarded master batch of content as 3: 2, then get the raw materials ready according to the proportioning in corresponding form, the component of getting ready stirs through high-speed mixer, evenly mixes; At last, the said mixture accurate measurement is sent in forcing machine, in the shearing of twin screw, is carried, mixing under, fully fusing, compound, then extrude through head, tie rod, pelletizing, drying is packaged as finished product at last.
The length-to-diameter ratio of double-screw extruder screw is 40, and front-end temperature is 180-190 ℃, and the stage casing temperature is 220-230 ℃, and the head extrusion temperature is 230 ℃, and screw speed is 100 rev/mins.
The fire retardant modified ABS resin of each embodiment and Comparative Examples preparation is injection molded into various standard Mechanics Performance Testing battens and colour table by the ASTM standard, and wherein the L value is used the test of COLOR-EYE 7000A spectrophotometer, and is as shown in table 1.
The corresponding table of table 1 physicals and testing method
| Physical property | Method of testing |
| Hot strength (50mm/min) | ASTM D638 |
| Bending strength (3mm/min) | ASTM D790 |
| Bending modulus (3mm/min) | ASTM D790 |
| IZOD notched Izod impact strength (3.2mm) | ASTM D256 |
| Flammability (vertical combustion 1.6mm) | UL 94 |
| The L value |
Embodiment 1
Embodiment 1 comprises embodiment 1-1 and 1-2, and its formula is as shown in table 2; Comparative Examples 1,2,3 formula are also as shown in table 2;
In table 2:
ABS resin is PA757, Taiwan CHIMEI company;
Brominated epoxy, bromine content 52%-55% opens and beautifies;
FR245, bromine content 67%, Shouguang, Shandong Wei Dong;
Antimonous oxide 1,0.8 μ m, the Hunan flash star;
Antimonous oxide 2,3.2 μ m, the Hunan flash star;
Zinc borate, 7 μ m, chemical industry is bored in east, Zibo;
Oxidation inhibitor is Irganox 1076, Ciba;
Photostabilizer is UVP, Ciba;
Anti-dripping agent is PTFE, and the Guangzhou entropy can Polymer Company;
Lubricate EBS (ethylene bis stearic acid amide), commercially available;
Black agglomerate: content of carbon black is 50%, and polyethylene wax is carrier, and is commercially available.
Embodiment 1-1,1-2 and Comparative Examples 1,2,3 performance test are as shown in table 3.
Table 2 embodiment 1-1,1-2 and Comparative Examples 1,2,3 formula table
| Embodiment 1-1 | Embodiment 1-2 | Comparative Examples 1 | Comparative Examples 2 | Comparative Examples 3 |
| ABS | 100 | 100 | 100 | 100 | 100 |
| Brominated epoxy | 21 | / | 21 | 20 | |
| FR245 | / | 20 | 20 | / | / |
| Antimonous oxide 1 | / | / | 7 | 7 | 7 |
| Antimonous oxide 2 | 5 | 5 | / | / | / |
| Zinc borate | 3 | 3 | / | / | / |
| Irganox 1076 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| UVP | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 |
| PTFE | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 |
| Black agglomerate | 3 | 3 | 3 | 3 | 3 |
| EBS | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 |
Table 3 embodiment 1-1,1-2 and Comparative Examples 1,2,3 performance test table
| Embodiment 1-1 | Embodiment 1-2 | Comparative Examples 1 | Comparative Examples 2 | Comparative Examples 3 | |
| Hot strength (MPa) | 39 | 41 | 42 | 41 | 44 |
| Bending strength (MPa) | 52 | 53 | 54 | 53 | 53 |
| Bending modulus (MPa) | 1910 | 2050 | 2080 | 2020 | 2040 |
| IZOD notched Izod impact strength (J/M) | 135 | 170 | 190 | 150 | 155 |
| Flame retardant rating (1.6mm) | V-0 | V-0 | V-0 | V-0 | V-1 |
| The L value | 27.6 | 27.3 | 28.2 | 28.6 | 28.3 |
Embodiment 2
Embodiment 2 comprises embodiment 2-1,2-2, and the formula of itself and Comparative Examples 4 is as shown in table 4;
Raw and auxiliary material is with embodiment 1, but the preparation method is the two step master batch methods of the above, but not the one-step technology in embodiment.Wherein inorganic fire-retarded master batch is the ABS carrier, and antimonous oxide 2 is respectively 15%, 10% with the content of zinc borate.
The performance test of embodiment 2-1,2-2 and Comparative Examples 4 is as shown in table 5.
The formula table of table 4 embodiment 2-1,2-2 and Comparative Examples 4
| Embodiment 2-1 | Embodiment 2-2 | Comparative Examples 4 | |
| ABS | 78.5 | 78.5 | 100 |
| FR245 | 20 | 19 | 19 |
| Inorganic fire-retarded master batch | 30 | 30 | / |
| Antimonous oxide 2 | / | / | 4.5 |
| Zinc borate | / | / | 3 |
| Irganox 1076 | 0.5 | 0.5 | 0.5 |
| UVP | 0.3 | 0.3 | 0.3 |
| PTFE | 0.3 | 0.3 | 0.3 |
| Black agglomerate | 3 | 3 | 3 |
| EBS | 1 | 1 | 1 |
The performance test table of table 5 embodiment 2-1,2-2,2-3 and Comparative Examples 4
| Embodiment 2-1 | Embodiment 2-2 | Comparative Examples 4 | |
| Hot strength (MPa) | 42 | 42 | 41 |
| Bending strength (MPa) | 53 | 54 | 52 |
| Bending modulus (MPa) | 2060 | 2080 | 2050 |
| IZOD notched Izod impact strength (J/M) | 175 | 180 | 172 |
| Flame retardant rating (1.6mm) | V-0 | V-0 | V-1 |
| The L value | 27.1 | 26.9 | 27.1 |
Embodiment 3
Embodiment 3 comprises embodiment 3-1,3-2,3-3 and 3-4, and its formula is as shown in table 6; Its preparation method such as embodiment 2.
Wherein:
Polyethylene wax, the Honeywell;
Oxidized polyethlene wax, the Honeywell;
Ethylene-vinyl acetate copolymer wax, the Honeywell;
Ethylene-acrylic acid copolymer wax; The Honeywell;
All the other supplementary materials are with embodiment 1.
The performance test of embodiment 3-1,3-2,3-3 and 3-4 is as shown in table 7.
The formula table of table 6 embodiment 3-1,3-2,3-3 and 3-4
| Embodiment 3-1 | Embodiment 3-2 | Embodiment 3-3 | Embodiment 3-4 | |
| ABS | 78.5 | 78.5 | 78.5 | 78.5 |
| FR245 | 19 | 19 | 19 | 19 |
| Inorganic fire-retarded master batch | 30 | 30 | 30 | 30 |
| Irganox 1076 | 0.5 | 0.5 | 0.5 | 0.5 |
| UVP | 0.3 | 0.3 | 0.3 | 0.3 |
| PTFE | 0.3 | 0.3 | 0.3 | 0.3 |
| Black agglomerate | 3 | 3 | 3 | 3 |
| Polyethylene wax | 0.6 | 0.4 | 0.6 | / |
| Oxidized polyethlene wax | / | / | / | 0.6 |
| Ethylene-vinyl acetate copolymer wax | 0.2 | 0.4 | / | 0.2 |
| Ethylene-acrylic acid copolymer wax | / | / | 0.2 | / |
The performance test table of table 7 embodiment 3-1,3-2,3-3 and 3-4
| Embodiment 3-1 | Embodiment 3-2 | Embodiment 3-3 | Embodiment 3-4 |
| Hot strength (MPa) | 42 | 42 | 42 | 42 |
| Bending strength (MPa) | 53 | 52 | 52 | 53 |
| Bending modulus (MPa) | 2060 | 2045 | 2060 | 2075 |
| IZOD notched Izod impact strength (J/M) | 182 | 176 | 190 | 184 |
| Flame retardant rating (1.6mm) | V-0 | V-0 | V-0 | V-0 |
| The L value | 26.2 | 26.5 | 26.4 | 26.5 |
Embodiment 4-7
A kind of fire retardant modified ABS resin of low-L value comprises following component and content (weight part):
Table 8, the component of the fire retardant modified ABS resin of low-L value and content (weight part)
| Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 | |
| ABS | 100 | 100 | 100 | 100 |
| Bromide fire retardant | Tetrabromo-bisphenol 10 | TDE 12 | Octabromodiphenyl ether 15 | Brominated epoxy 10/ hexabromobenzene 5/ PHT4 10 |
| Inorganic fire-retarded master batch | 20 | 30 | 35 | 40 |
| Irganox 168 | 1 | 0.8 | 0.5 | 0.2 |
| Photostabilizer | 2-dihydroxy benaophenonel 0.1 | Diphenyl phosphite 0.3 | Triphenyl phosphite 0.4 | Hydroxybenzotriazole 0.5 |
| PTFE | 0.5 | 0.3 | 0.2 | 0.1 |
| Black agglomerate | 4 | 3 | 3 | 1 |
| Lubricant | Silicone oil 1/ paraffin 2 | White mineral oil 1.5 | Magnesium Stearate 2.5 | Fatty acid amide 1 |
Described inorganic fire-retarded master batch is take ABS resin as carrier, load Sb system fire retardant and zinc borate, and wherein take the weight of inorganic fire-retarded master batch as 100%, the component of Sb system fire retardant and zinc borate and the weight percentage that accounts for inorganic fire-retarded master batch see Table 9; Black agglomerate is the complex body take polyolefine or ethylene-vinyl acetate copolymer as carrier loaded carbon black, and described content of carbon black is 20-60wt%, and described polyolefinic molecular weight is 2000-10000.
Table 9
The preparation method of the fire retardant modified ABS resin of above-mentioned low-L value comprises the following steps:
(1) get the raw materials ready according to upper table 9 component and content:
(2) use twin screw extruder, take Sb system fire retardant and zinc borate as raw material, the inorganic fire-retarded master batch of preparation take ABS resin as carrier;
(3) the inorganic fire-retarded master batch and the ABS resinoid that step (2) are obtained, after bromide fire retardant, anti-dripping agent, oxidation inhibitor, photostabilizer, lubricant, black agglomerate stir in high-speed mixer and fully mix, send in twin screw extruder through measuring apparatus, the conveying of screw rod, shearing and mixing under, material melting, compound, again through extrude, tie rod, cooling, pelletizing step, obtain the fire retardant modified ABS resin of low-L value.
The screw slenderness ratio of described twin screw extruder is 40, and with temperature control unit and vacuum extractor; The extrusion temperature of described extrusion step is between 190-230 ℃, and screw speed is 100-300 rev/min.
Claims (2)
1. the fire retardant modified ABS resin of a low-L value, is characterized in that, this resin is prepared from by following component and weight part content:
Described ABS resinoid is acrylonitrile-butadiene-styrene copolymer, acrylonitrile-butadiene-acrylate copolymer, MBS or vinyl cyanide-terpolymer EP rubber-styrol copolymer;
Described bromide fire retardant is one or several the mixture in tetrabromo-bisphenol, TDE, three (bromophenyl) triazine, brominated epoxy, decabromodiphenyl oxide, hexabromocyclododecane, PHT4, hexabromobenzene, octabromodiphenyl ether or Brominated Polystyrene; Described inorganic fire-retarded master batch is take ABS resin as carrier, load Sb system fire retardant 5-30wt% and zinc borate 5-30wt%;
Described Sb system fire retardant is a kind of in antimonous oxide, antimony peroxide or sodium antimonate;
Described anti-dripping agent is that molecular weight is 3,000,000-5,000,000 tetrafluoroethylene;
Described oxidation inhibitor is refine Irganox 1010, the Irganox 1076 of company or one or several the mixture in Irganox 168 of CIBA; Described photostabilizer is one or several the mixture in 2-dihydroxy benaophenonel, salicylate class, diphenyl phosphite, triphenyl phosphite or hydroxybenzotriazole; Described lubricant is one or several the mixture in silicone oil, white mineral oil, fatty acid amide, barium stearate, Magnesium Stearate, paraffin, polyethylene wax, ethylene bis stearic acid amide, ethylene-vinyl acetate copolymer or ethylene-acrylic acid copolymer;
Described black agglomerate is the complex body take polyolefine or ethylene-vinyl acetate copolymer as carrier loaded carbon black, and described content of carbon black is 20-60wt%, and described polyolefinic molecular weight is 2000-10000.
2. the preparation method of the fire retardant modified ABS resin of a low-L value as claimed in claim 1, is characterized in that, the method comprises the following steps:
(1) get the raw materials ready according to following component and weight part content:
(2) use twin screw extruder, take Sb system fire retardant and zinc borate as raw material, the inorganic fire-retarded master batch of preparation take ABS resin as carrier;
(3) after the inorganic fire-retarded master batch that step (2) is obtained stirs in high-speed mixer with ABS resinoid, bromide fire retardant, anti-dripping agent, oxidation inhibitor, photostabilizer, lubricant, black agglomerate and fully mixes, send in twin screw extruder through measuring apparatus, the conveying of screw rod, shearing and mixing under, material melting, compound, again through extrude, tie rod, cooling, pelletizing step, obtain the fire retardant modified ABS resin of low-L value;
In described inorganic fire-retarded master batch, the weight content of Sb system fire retardant and zinc borate is 5%-30%;
The screw slenderness ratio of described twin screw extruder is 40, and with temperature control unit and vacuum extractor; The extrusion temperature of described extrusion step is between 190-230 ℃, and screw speed is 100-300 rev/min.
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| WO2021177199A1 (en) * | 2020-03-06 | 2021-09-10 | 三菱エンジニアリングプラスチックス株式会社 | Resin composition, molded article, and electric wire |
| CN111846674A (en) * | 2020-08-19 | 2020-10-30 | 江苏翔云航空设备零部件有限公司 | Separated-bin type explosion-proof functional structural body |
| CN112480594B (en) * | 2020-11-27 | 2022-08-09 | 天津金发新材料有限公司 | High-black flame-retardant ABS (acrylonitrile-butadiene-styrene) compound with extinction effect and preparation method and application thereof |
| CN113881183B (en) * | 2021-11-09 | 2023-10-20 | 广东锦湖日丽高分子材料有限公司 | Flame-retardant ABS resin composition with low infrared reflectivity and preparation method thereof |
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2009
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