CN103509309A - Environment-friendly low-smoke fire-retardant acrylonitrile-butadiene-styrene (ABS) resin and preparation method thereof - Google Patents
Environment-friendly low-smoke fire-retardant acrylonitrile-butadiene-styrene (ABS) resin and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of fire-retardant resins, and discloses an acrylonitrile-butadiene-styrene (ABS) resin and a preparation method thereof. The resin is prepared from the following components in parts by weight: 1000 parts of ABS resin, 150-350 parts of halogen flame retardants, 30-70 parts of synergistic fire retardant, 30-70 parts of smoke suppressant, 1-10 parts of antioxidant, and 1-10 parts of lubricant. The preparation method comprises the following steps: fully and evenly mixing the 1000 parts of ABS resin, 150-350 parts of halogen flame retardants, 30-70 parts of synergistic fire retardant, 30-70 parts of smoke suppressant, 1-10 parts of antioxidant and 1-10 parts of lubricant; feeding the materials to a double-screw extruder through a precise metering feeder after completely mixing; fully fusing the materials under the conditions of shearing, mixing and conveying of screws; and finally preparing granules after extruding, bracing and cooling. The ABS resin disclosed by the invention is low in smoke generation in combustion, does not generate harmful gases such as dioxin, does not generate molten droplets, accords with the instruction of restriction of hazardous substances (ROHS) of the European Union, and is low in cost and convenient to process.
Description
Technical field
The present invention relates to flame-retarded resin technical field, relate to a kind of environmental protection low-smoke flame-proof ABS resinoid and preparation method thereof.
Background technology
Acrylonitrile-butadiene-styrene terpolymer (ABS) is a kind of common resins for universal use, ABS over-all properties is good, high tenacity, easily electroplate painted, and easily processing, be widely used in the industries such as automobile, household electrical appliances, electronic apparatus, machinery, and along with the demand of the development ABS of modern science and technology is also increasing fast, current output comes the 5th of resin yield.Although ABS has a lot of advantages, but still there are some defects, for example, poor fire, oxygen index is only 18-20, vertical combustion is only the HB level of UL94 standard.Poor fire has restricted the development of ABS, because the fire of the inflammable initiation of plastics, cause the poison gas of fire enlarged areas, release to cause the accidents such as loss of life and personal injury can be found everywhere, therefore the research and development of flame-proof ABS become a large study hotspot, through development for many years, flame-proof ABS system reaches its maturity, and halogen-antimony synergistic system becomes a classical case of flame-retarded resin technology.The shortcoming that but flame-proof ABS still has, and the amount of being fuming is large, poison gas is heavy.
Hydrotalcite is the novel layer silicate mineral of a class, is mainly used in acid-acceptor and PVC stablizer.Hydrotalcite when being heated water of constitution laminated sheet hydroxyl and interlayer ion with water and CO
2form deviate from, can play and reduce combustion gases concentration, intercept O
2fire retardation, and its decomposes product is that alkaline many empties matter specific surface area is large, can absorb obnoxious flavour and suspended particle, in hydrotalcite, distinctive metal radical ion can generate halogenide and cover the effect that material surface plays starvation in combustion processes simultaneously, therefore the fire-retardant ABS of halogen-antimony is had good fire-retardant synergistic and presses down cigarette effect.Current low-smoke flame-proof ABS, the smoke suppressant of using mostly is the molybdenum compound of molybdenum oxide, ammonium molybdate or zinc molybdate one class, expensive, sharp hydrotalcite reduces the cost that the flame-proof ABS amount of being fuming can effectively reduce flame-proof ABS, has to have that raw cigarette amount is low, the feature of good flame retardation effect.
Summary of the invention
Deficiency and defect for existing flame retardant ABS resin technology, the object of this invention is to provide a kind of environmental protection low-smoke flame-proof ABS resinoid, this flame retardant ABS resin when burning the amount of being fuming low, do not produce the obnoxious flavoures such as dioxin, do not produce melting drippage, meet the ROHS of European Union instruction, and cost is low, easy to process.
Another object of the present invention is to provide the resinoid preparation method of a kind of above-mentioned ABS.
For achieving the above object, the technical solution used in the present invention is as follows:
The invention provides a kind of environmental protection low-smoke flame-proof ABS resinoid, this resin is made by the component that comprises following weight part:
1000 parts of ABS resinoids,
150 ~ 350 parts of halogenated flame retardants,
30 ~ 70 parts of synergistic flame retardants,
30 ~ 70 parts of smoke suppressants,
1 ~ 10 part, oxidation inhibitor,
1 ~ 10 part of lubricant.
The present invention further provides a kind of environmental protection low-smoke flame-proof ABS resinoid, this resin is made by the component that comprises following weight part:
1000 parts of ABS resinoids,
180 ~ 300 parts of halogenated flame retardants,
40 ~ 60 parts of synergistic flame retardants,
40 ~ 60 parts of smoke suppressants,
3 ~ 8 parts, oxidation inhibitor,
3 ~ 5 parts of lubricants.
Described ABS resinoid is selected from one or more in acrylonitrile-butadiene-styrene terpolymer (ABS) or acrylonitritrile-styrene resin (AS).
Described halogenated flame retardant is selected from one or more in chlorinatedpolyethylene, tetrafluoroethylene, TDE, brominated epoxy resin, brominated Polystyrene, tetrabromo-bisphenol, brominated triazine or bromophenisic acid isocyanic ester.
Described synergistic flame retardant is antimonous oxide (Sb
2o
3) and the compound of humite, its ratio is 3:1 ~ 1:1.
Described smoke suppressant is selected from magnesium-aluminum-based hydrotalcite.
Described magnesium-aluminum-based hydrotalcite is selected from one or more in borate intercalation magnesium-aluminum-based hydrotalcite, phosphate radical intercalation magnesium-aluminum-based hydrotalcite or stearate radical intercalation magnesium-aluminum-based hydrotalcite.
Described oxidation inhibitor is Hinered phenols antioxidant.
Described Hinered phenols antioxidant is selected from 2, 6-di-tert-butyl-4-methy phenol, β-(4 '-hydroxyl-3 ', 5 '-di-tert-butyl-phenyl) vinylformic acid octadecyl ester (antioxidant 1076), β-(3, 5-di-t-butyl hydroxy phenyl) vinylformic acid ten caprylates, triphenyl phosphite, trisnonylphenyl phosphite, three (2, 4-tert-butyl-phenyl) phosphorous acid ester (irgasfos 168), four [methylene radical-3,-3 ', 5-(di-t-butyl-4-hydroxyl-phenyl) vinylformic acid] methane or 3, 9-two [1, 1-dimethyl-2-[(3-tertiary butyl-4-hydroxy-5-aminomethyl phenyl) propionyloxy] ethyl]-2, 4, 8, one or more in 10-tetra-oxaspiros [5.5] undecane (oxidation inhibitor AO80).
Described lubricant is selected from stearic acid, calcium stearate, barium stearate, N, one or more in N '-ethylene bis stearamide (EBS), polyethylene wax or methyl-silicone oil.
The present invention also provides a kind of preparation method of above-mentioned flame retardant ABS resin, and the method comprises the following steps:
1000 parts of ABS resinoids, 150 ~ 350 parts of halogenated flame retardants, 30 ~ 70 parts of synergistic flame retardants, 30 ~ 70 parts of smoke suppressants, 1 ~ 10 part of oxidation inhibitor and 1 ~ 10 part of lubricant are fully mixed, after mixing completely; By the pay-off of delicate metering, material is sent in twin screw extruder, material the shearing of screw rod, mixing and carry under fusion fully, finally by crossing, extrude, tie rod, cooling after, make pellet.
The length-to-diameter ratio of described twin screw extruder is 20:1 ~ 60:1, and with the twin screw extruder of accurate temperature control and vacuum-pumping equipment, the temperature setting in each district of screw rod is set to 170 ~ 230 ℃.
The present invention compared with prior art, has the following advantages and beneficial effect:
The present invention utilizes hydrotalcite for smoke suppressant, does not affect flowing property and the processing characteristics of ABS material, applicable to extruding and injection moulding.Hydrotalcite when being heated water of constitution laminated sheet hydroxyl and interlayer ion with water and CO
2form deviate from, can play and reduce combustion gases concentration, intercept O
2fire retardation, and its decomposes product is that alkaline many empties matter specific surface area is large, can absorb obnoxious flavour and suspended particle, in hydrotalcite, distinctive metal radical ion can generate halogenide and cover the effect that material surface plays starvation in combustion processes simultaneously, therefore the fire-retardant ABS of halogen-antimony there is is good fire-retardant synergistic and presses down cigarette effect, in the present invention, preferred borate intercalation magnesium-aluminum-based hydrotalcite, phosphate radical intercalation magnesium-aluminum-based hydrotalcite or stearate radical intercalation magnesium-aluminum-based hydrotalcite are as smoke suppressant, and its effect is more outstanding.
Meanwhile, this flame-proof ABS is still used halogen antimony synergistic system fire-retardant, can guarantee the flame retardant effect of material, can test by ROHS, and the amount of being fuming while simultaneously having reduced material combustion, and with low cost.Guaranteeing, under the prerequisite of flame retardant effect, not reduce the mechanical property of material, there is the good market space.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
ABS(Jin Hu, 750N) 1000 parts,
100 parts of chlorinatedpolyethylenees,
200 parts of brominated epoxy resins,
Sb
2o
320 parts,
20 parts of humites,
60 parts of borate intercalation magnesium-aluminum-based hydrotalcites,
107 2 parts, oxidation inhibitor,
3 parts of irgasfos 168s,
5 parts of calcium stearates;
According to the weight part that feeds intake of above-mentioned material, ABS resinoid, halogenated flame retardant, synergistic flame retardant, smoke suppressant, oxidation inhibitor and lubricant add in homogenizer and fully mix, after mixing completely; By the pay-off of delicate metering, material is sent in twin screw extruder, wherein the length-to-diameter ratio of twin screw extruder is 45:1, twin screw extruder with accurate temperature control and vacuum-pumping equipment, the temperature setting in each district of screw rod is set to 180-210 ℃, material the shearing of screw rod, mixing and carry under fusion fully, finally by crossing, extrude, tie rod, cooling after, make pellet, its mechanical property refers to table 1.
Embodiment 2
ABS(Gaoqiao Petrochemical Company, 8434) 1000 parts,
250 parts of tetrabromo-bisphenols,
Sb
2o
345 parts,
15 parts of humites,
40 parts of phosphate radical intercalation magnesium-aluminum-based hydrotalcites,
107 63 parts, oxidation inhibitor,
5 parts of oxidation inhibitor AO80,
4 parts of EBS;
According to the weight part that feeds intake of above-mentioned material, ABS resinoid, halogenated flame retardant, synergistic flame retardant, smoke suppressant, oxidation inhibitor and lubricant add in homogenizer and fully mix, after mixing completely; By the pay-off of delicate metering, material is sent in twin screw extruder, and wherein the length-to-diameter ratio of twin screw extruder is 45:1, with the twin screw extruder of accurate temperature control and vacuum-pumping equipment, the temperature setting in each district of screw rod is set to 170-200 ℃, and its mechanical property refers to table 1.
Embodiment 3
ABS(Gaoqiao Petrochemical Company, 8434) 1000 parts,
150 parts of TDE,
Sb
2o
330 parts,
10 parts of humites,
50 parts of stearate radical intercalation magnesium-aluminum-based hydrotalcites,
107 62 parts, oxidation inhibitor,
4 parts of irgasfos 168s,
5 parts of stearic acid;
According to the weight part that feeds intake of above-mentioned material, ABS resinoid, halogenated flame retardant, synergistic flame retardant, smoke suppressant, oxidation inhibitor and lubricant add in homogenizer and fully mix, after mixing completely; By the pay-off of delicate metering, material is sent in twin screw extruder, and wherein the length-to-diameter ratio of twin screw extruder is 45:1, with the twin screw extruder of accurate temperature control and vacuum-pumping equipment, the temperature setting in each district of screw rod is set to 180-210 ℃, and its mechanical property refers to table 1.
Embodiment 4
ABS(Jin Hu, 750) 1000 parts,
220 parts of brominated triazines,
Sb
2o
330 parts,
20 parts of humites,
40 parts of borate intercalation magnesium-aluminum-based hydrotalcites,
107 61 parts, oxidation inhibitor,
2 parts of oxidation inhibitor AO80
3 parts of polyethylene waxs;
According to the weight part that feeds intake of above-mentioned material, ABS resinoid, halogenated flame retardant, synergistic flame retardant, smoke suppressant, oxidation inhibitor and lubricant add in homogenizer and fully mix, after mixing completely; By the pay-off of delicate metering, material is sent in twin screw extruder, and wherein the length-to-diameter ratio of twin screw extruder is 45:1, with the twin screw extruder of accurate temperature control and vacuum-pumping equipment, the temperature setting in each district of screw rod is set to 200-230 ℃, and its mechanical property refers to table 1.
Embodiment 5
ABS(Jin Hu, 750) 1000 parts,
280 parts of brominated triazines,
Sb
2o
340 parts,
20 parts of humites,
50 parts of borate intercalation magnesium-aluminum-based hydrotalcites,
107 62 parts, oxidation inhibitor,
4 parts of irgasfos 168s,
5 parts of EBS;
According to the weight part that feeds intake of above-mentioned material, ABS resinoid, halogenated flame retardant, synergistic flame retardant, smoke suppressant, oxidation inhibitor and lubricant add in homogenizer and fully mix, after mixing completely; By the pay-off of delicate metering, material is sent in twin screw extruder, and wherein the length-to-diameter ratio of twin screw extruder is 45:1, with the twin screw extruder of accurate temperature control and vacuum-pumping equipment, the temperature setting in each district of screw rod is set to 180-210 ℃, and its mechanical property refers to table 1.
Comparative example
ABS(Jin Hu, 750N) 1000 parts,
250 parts of brominated triazines,
Sb
2o
370 parts,
1 part of antioxidant 1076,
2 parts of irgasfos 168s,
3 parts of EBS;
The weight part that feeds intake according to above-mentioned material, adds each component materials in homogenizer and fully mixes, after mixing completely; By the pay-off of delicate metering, material is sent in twin screw extruder, wherein the length-to-diameter ratio of twin screw extruder is 45:1, and the temperature setting in each district of screw rod is set to 180-210 ℃, and its mechanical property refers to table 1.
Embodiment 6
AS(Jin lake, 80HF) 600 parts,
ABS(Jin Hu, 181H) 400 parts,
350 parts of brominated Polystyrenes,
Sb
2o
350 parts,
20 parts of humites,
70 parts of borate intercalation magnesium-aluminum-based hydrotalcites,
4 parts of antioxidant 1076s,
6 parts of irgasfos 168s,
10 parts of EBS;
According to the weight part that feeds intake of above-mentioned material, AS, halogenated flame retardant, synergistic flame retardant, smoke suppressant, oxidation inhibitor and lubricant add in homogenizer and fully mix, after mixing completely; By the pay-off of delicate metering, material is sent in twin screw extruder, and wherein the length-to-diameter ratio of twin screw extruder is 45:1, with the twin screw extruder of accurate temperature control and vacuum-pumping equipment, the temperature setting in each district of screw rod is set to 180-210 ℃, and its mechanical property refers to table 1.
Embodiment 7
ABS(Gaoqiao Petrochemical Company 8391) 1000 parts,
180 parts of bromophenisic acid isocyanic ester,
Sb
2o
350 parts,
20 parts of humites,
70 parts of borate intercalation magnesium-aluminum-based hydrotalcites,
0.5 part of antioxidant 1076,
0.5 part of irgasfos 168,
1 part of EBS;
According to the weight part that feeds intake of above-mentioned material, AS, halogenated flame retardant, synergistic flame retardant, smoke suppressant, oxidation inhibitor and lubricant add in homogenizer and fully mix, after mixing completely; By the pay-off of delicate metering, material is sent in twin screw extruder, wherein the length-to-diameter ratio of twin screw extruder is 45:1, with the twin screw extruder of accurate temperature control and vacuum-pumping equipment, the temperature setting in each district of screw rod is set to 180-210 ℃.
Table 1
| ASTM | Melting index g/10min | Notched Izod impact strength KJ/m 2 | UL94 flame retardant properties | Smoke density (Dm) |
| Embodiment 1 | 58 | 18 | 3.2mmV01.6mmHB | 180 |
| Embodiment 2 | 80 | 15 | 3.2mmV01.6mmHB | 200 |
| Embodiment 3 | 32 | 12 | 3.2mmV01.6mmV1 | 200 |
| Embodiment 4 | 55 | 14 | 3.2mmV01.6mmHB | 220 |
| Embodiment 5 | 50 | 12 | 3.2mmV01.6mmV0 | 195 |
| Embodiment 6 | 37 | 14 | 3.2mmV01.6mmV1 | 225 |
| Embodiment 7 | 43 | 20 | 3.2mmV01.6mmHB | 190 |
| Comparative example | 48 | 14 | 3.2mmV01.6mmV2 | 350 |
As shown in Table 1, raw cigarette in the time of effectively reducing flame-proof ABS burning with hydrotalcite as smoke suppressant, and kept good impact property and flame retardant properties, because the price of commercially available hydrotalcite obtains smoke suppressant far below molybdenum compound class, so this patent has good development prospect.
Embodiment 8
1000 parts of ABS, 200 parts of tetrafluoroethylene, 20 parts of Sb
2o
3, 10 parts of humites, 7 parts of borate intercalation magnesium-aluminum-based hydrotalcites, 3 part 2,6-di-tert-butyl-4-methy phenol, 2 portions of triphenyl phosphites, 2 parts of trisnonylphenyl phosphites, 3 parts of barium stearates and 4 parts of methyl-silicone oils add in homogenizer and fully mix, after mixing completely; By the pay-off of delicate metering, material is sent in twin screw extruder, wherein the length-to-diameter ratio of twin screw extruder is 45:1, with the twin screw extruder of accurate temperature control and vacuum-pumping equipment, the temperature setting in each district of screw rod is set to 180-210 ℃.
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.Person skilled in the art obviously can easily make various modifications to these embodiment, and General Principle described herein is applied in other embodiment and needn't passes through performing creative labour.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, and not departing from the improvement that category of the present invention makes and revise all should be within protection scope of the present invention.
Claims (10)
1. an ABS resinoid, is characterized in that: this resin is made by the component that comprises following weight part:
1000 parts of ABS resinoids,
150 ~ 350 parts of halogenated flame retardants,
30 ~ 70 parts of synergistic flame retardants,
30 ~ 70 parts of smoke suppressants,
1 ~ 10 part, oxidation inhibitor,
1 ~ 10 part of lubricant.
2. ABS resinoid according to claim 1, is characterized in that: this resin is made by the component that comprises following weight part:
1000 parts of ABS resinoids,
180 ~ 300 parts of halogenated flame retardants,
40 ~ 60 parts of synergistic flame retardants,
40 ~ 60 parts of smoke suppressants,
3 ~ 8 parts, oxidation inhibitor,
3 ~ 5 parts of lubricants.
3. ABS resinoid according to claim 1, is characterized in that: described ABS resinoid is selected from one or more in acrylonitrile-butadiene-styrene terpolymer or acrylonitritrile-styrene resin.
4. ABS resinoid according to claim 1, is characterized in that: described halogenated flame retardant is selected from one or more in chlorinatedpolyethylene, tetrafluoroethylene, TDE, brominated epoxy resin, brominated Polystyrene, tetrabromo-bisphenol, brominated triazine or bromophenisic acid isocyanic ester; Described synergistic flame retardant is the compound of antimonous oxide and humite, and its ratio is 3:1 ~ 1:1.
5. ABS resinoid according to claim 1, is characterized in that: described smoke suppressant is selected from magnesium-aluminum-based hydrotalcite.
6. ABS resinoid according to claim 5, is characterized in that: described magnesium-aluminum-based hydrotalcite is selected from one or more in borate intercalation magnesium-aluminum-based hydrotalcite, phosphate radical intercalation magnesium-aluminum-based hydrotalcite or stearate radical intercalation magnesium-aluminum-based hydrotalcite.
7. ABS resinoid according to claim 1, is characterized in that: described oxidation inhibitor is Hinered phenols antioxidant.
8. ABS resinoid according to claim 7, it is characterized in that: described Hinered phenols antioxidant is selected from 2, 6-di-tert-butyl-4-methy phenol, β-(4 '-hydroxyl-3 ', 5 '-di-tert-butyl-phenyl) vinylformic acid octadecyl ester, β-(3, 5-di-t-butyl hydroxy phenyl) vinylformic acid ten caprylates, triphenyl phosphite, trisnonylphenyl phosphite, three (2, 4-tert-butyl-phenyl) phosphorous acid ester, four [methylene radical-3,-3 ', 5-(di-t-butyl-4-hydroxyl-phenyl) vinylformic acid] methane or 3, 9-two [1, 1-dimethyl-2-[(3-tertiary butyl-4-hydroxy-5-aminomethyl phenyl) propionyloxy] ethyl]-2, 4, 8, one or more in 10-tetra-oxaspiros [5.5] undecane.
9. ABS resinoid according to claim 1, is characterized in that: described lubricant is selected from stearic acid, calcium stearate, barium stearate, N one or more in N '-ethylene bis stearamide, polyethylene wax or methyl-silicone oil.
10. the arbitrary described resinoid preparation method of ABS of claim 1 to 8, is characterized in that: the method comprises the following steps:
1000 parts of ABS resinoids, 150 ~ 350 parts of halogenated flame retardants, 30 ~ 70 parts of synergistic flame retardants, 30 ~ 70 parts of smoke suppressants, 1 ~ 10 part of oxidation inhibitor and 1 ~ 10 part of lubricant are fully mixed, after mixing completely; By the pay-off of delicate metering, material is sent in twin screw extruder, material the shearing of screw rod, mixing and carry under fusion fully, finally by crossing, extrude, tie rod, cooling after, make pellet;
The length-to-diameter ratio of described twin screw extruder is 20:1 ~ 60:1, and with the twin screw extruder of accurate temperature control and vacuum-pumping equipment, the temperature setting in each district of screw rod is set to 170 ~ 230 ℃.
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| CN109111677B (en) * | 2018-07-17 | 2021-03-19 | 广东聚石化学股份有限公司 | Low-smoke-density UL94-5 VA-grade flame-retardant ABS material and preparation method thereof |
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| CN114806071A (en) * | 2022-05-27 | 2022-07-29 | 史凤华 | Environment-friendly flame-retardant anti-aging ABS composite material and preparation method thereof |
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Application publication date: 20140115 |