CN111019287A - Graphene synergistic flame-retardant ABS/SBS composite material and preparation method thereof - Google Patents

Graphene synergistic flame-retardant ABS/SBS composite material and preparation method thereof Download PDF

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CN111019287A
CN111019287A CN201911365803.6A CN201911365803A CN111019287A CN 111019287 A CN111019287 A CN 111019287A CN 201911365803 A CN201911365803 A CN 201911365803A CN 111019287 A CN111019287 A CN 111019287A
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flame
retardant
composite material
sbs
parts
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CN111019287B (en
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王立春
孙青�
缪爱东
张伟
张瑜
黄南婷
柏璐
李海洋
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Jiangsu Shenghe New Material Technology Co ltd
Nantong University
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Nantong University
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L55/00—Compositions of homopolymers or copolymers, obtained by polymerisation reactions only involving carbon-to-carbon unsaturated bonds, not provided for in groups C08L23/00 - C08L53/00
    • C08L55/02—ABS [Acrylonitrile-Butadiene-Styrene] polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/32—Phosphorus-containing compounds
    • C08K2003/321—Phosphates
    • C08K2003/322—Ammonium phosphate
    • C08K2003/323—Ammonium polyphosphate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/02—Flame or fire retardant/resistant
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/06—Polymer mixtures characterised by other features having improved processability or containing aids for moulding methods
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers

Abstract

The invention discloses a graphene synergistic flame-retardant ABS/SBS composite material and a preparation method thereof. The composite material is prepared by adopting ABS resin as a basic material, adding a toughening agent, a compatibilizer, a flame retardant, a synergistic flame retardant, a dispersing agent, a lubricant and an antioxidant, fully mixing by a high-speed mixer, and then performing double-screw melt extrusion granulation. According to the invention, the SBS elastomer material is added as the toughening agent, so that the toughness and low temperature resistance of the ABS material are improved; by adding the flame-retardant synergist graphene, a flame-retardant composite system is formed with the polyphosphate flame retardant, so that the flame-retardant efficiency is improved, and the tensile strength and toughness of the ABS material are effectively improved or maintained. The flame-retardant ABS/SBS composite material prepared by the invention has the characteristics of good flame retardance, no precipitation, high toughness, low temperature resistance and the like.

Description

Graphene synergistic flame-retardant ABS/SBS composite material and preparation method thereof
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a graphene synergistic flame-retardant ABS/SBS composite material and a preparation method thereof.
Background
ABS plastics are terpolymers of acrylonitrile-butadiene-styrene, and are widely applied in the fields of electronic and electric appliances, transportation, instruments and meters, medical care and the like due to the characteristics of easy availability of raw materials, good comprehensive performance, high cost performance, easy molding and processing and the like. But the flame retardance is not high, the impact strength at low temperature is poor, and the like, and the application range of the flame-retardant polypropylene composite material is limited to a certain extent. Therefore, when the flame retardant is used in occasions with higher flame retardant requirements and low temperature resistance, modification is required to improve the flame retardant property and the low temperature impact strength.
Disclosure of Invention
In order to meet and expand the application of ABS plastics in the fields of electronic industry and the like, which have the requirements of higher flame retardance, low temperature resistance and the like, the invention provides a graphene synergistic flame-retardant ABS/SBS composite material.
In order to achieve the purpose, the invention adopts the following technical scheme:
the graphene synergistic flame-retardant ABS/SBS composite material comprises the following raw materials in parts by weight: 100 parts of ABS resin, 0-100 parts of toughening agent SBS and compatibilizer SBS-g-NH20-15 parts of a flame retardant, 10-60 parts of a flame retardant synergist, 0-8 parts of a flame retardant synergist, 0-2 parts of a dispersing agent, 0.1-3 parts of a lubricant and 0.1-2 parts of an antioxidant.
Further, the melt index of the ABS resin is more than or equal to 15g/10min (220 ℃/10kg), and the specific gravity of the ABS resin is 1.05g/cm3Tensile strength is more than or equal to 40MPa, and IZOD (23 ℃) notch impact strength is more than or equal to 20KJ/m2The IZOD (-40 ℃) notch impact strength is more than or equal to 8.5KJ/m2. Preferably, the melt index of the ABS resin is more than or equal to 20g/10min (220 ℃/10kg), the tensile strength is more than or equal to 45MPa, and the IZOD (-40 ℃) notch impact strength is more than or equal to 10KJ/m2。
Further, the compatibilizer SBS-g-NH2，NH2The grafting ratio of (A) is 0.1-2.5%.
Further, the flame retardant is polyphosphate or phosphate flame retardant selected from melamine polyphosphate (MPP), ammonium polyphosphate (APP), triphenyl phosphate (TPP) or resorcinol bis (diphenyl phosphate) (RDP). Preferably, the flame retardants are phosphorus/nitrogen element-containing polyphosphates MPP and APP.
Further, the flame-retardant synergist is graphene, and the single-layer rate of the flame-retardant synergist is more than or equal to 60%. Preferably, the flame retardant synergist is lipophilic graphene powder, the number of layers (thickness) of the flame retardant synergist is 1-3, the single-layer rate is more than 80%, the carbon content is more than or equal to 98%, the sheet diameter (D50) is 4-7 μm, the sheet diameter (D90) is 9-11 μm, the average diameter-thickness ratio is 8500, the flame retardant synergist is black-gray powder, and the bulk density is 0.01-0.02 g/mL.
Further, the dispersant is a sodium polyacrylate anionic dispersant.
Further, the lubricant is E wax.
Further, the antioxidant is a hindered phenol antioxidant selected from the group consisting of antioxidant 1010, antioxidant 1076 and antioxidant 1098.
The preparation method of the graphene synergistic flame-retardant ABS/SBS composite material comprises the steps of preparing ABS resin, a toughening agent SBS and a compatibilizer SBS-g-NH2The flame retardant, the flame-retardant synergist, the dispersing agent, the lubricant and the antioxidant are sequentially added into a high-speed mixer, fully mixed for 5-6 min and then extruded by a double-screw extruderAnd (3) performing melt extrusion granulation at 230-280 ℃ to obtain the composite material.
Further, the length-diameter ratio (L/D) of the double-screw extruder is 35-52. Preferably, L/D is 42.
The invention adopts ABS resin with excellent comprehensive performance as basic material, improves the toughness, low temperature resistance and processability of the ABS material by adding SBS elastomer material, and improves the toughness, low temperature resistance and processability of the ABS material by adding compatibilizer SBS-g-NH2The compatibility of the ABS/SBS blend is increased.
According to the invention, the flame-retardant synergist graphene is added to form a flame-retardant composite system with the polyphosphate flame retardant, so that the efficiency of the flame retardant is greatly improved, and the tensile strength and the impact resistance of the ABS material are effectively maintained or improved.
Detailed Description
The preparation method of the graphene synergistic flame-retardant ABS/SBS composite material provided by the invention comprises the steps of mixing 100 parts of ABS resin, 0-100 parts of toughening agent SBS and 0-15 parts of compatibilizer SBS-g-NH2(amino grafted SBS), 10-60 parts of flame retardant, 0-8 parts of flame retardant synergist, 0-2 parts of dispersing agent, 0.1-3 parts of lubricating agent and 0.1-2 parts of antioxidant are sequentially added into a high-speed mixer, fully mixed for 5-6 min, and then subjected to melt extrusion granulation at 230-280 ℃ through a double-screw extruder to obtain the graphene synergistic flame retardant ABS/SBS composite material.
The ABS resin adopted by the invention is yellowish granular, the melt index is more than or equal to 15g/10min (220 ℃/10kg), and the specific gravity is 1.05g/cm3Tensile strength is more than or equal to 40MPa, and IZOD (23 ℃) notch impact strength is more than or equal to 20KJ/m2The IZOD (-40 ℃) notch impact strength is more than or equal to 8.5KJ/m2. The preferable ABS resin has a melt index of more than or equal to 20g/10min (220 ℃/10kg), a tensile strength of more than or equal to 45MPa, and an IZOD (-40 ℃) notch impact strength of more than or equal to 10KJ/m2。
The toughening agent adopted by the invention is SBS which is produced by Asahi Kasei Corp, the brand is P2000, the hardness is 74D, the S/B is 67/33, the tensile strength is 24.5MPa, the elongation at break is 42 percent, the melt index is 3.0g/10min (190 ℃/2.16KG), and the specific gravity is 0.98g/cm3。
Produced by the inventionThe compatibilizer used is SBS grafted by amino (SBS-g-NH)2) In which NH2The grafting ratio of (A) is 0.1-2.5%. Preferred SBS-g-NH2The trade name is MP10 manufactured by Asahi Kasei corporation, Japan, NH thereof2The graft ratio of (A) was 1.8%, the Shore hardness was 89A, the S/B was 30/70, the tensile strength was 28MPa, the elongation at break was 600%, the melt index was 4.0g/10min (190 ℃/2.16KG), and the specific gravity was 0.91g/cm3。
The flame retardant used in the invention is polyphosphate or phosphate flame retardant, such as melamine polyphosphate (MPP), ammonium polyphosphate (APP), triphenyl phosphate (TPP), resorcinol bis (diphenyl phosphate) (RDP) and the like. The preferable flame retardant is polyphosphate MPP and APP containing phosphorus/nitrogen elements, wherein the flame retardant is MPP and white powder, the phosphorus content is more than or equal to 13 percent, the nitrogen content is more than or equal to 37 percent, the fineness (30 mu m) is more than or equal to 99 percent, the thermal decomposition temperature is more than or equal to 300 ℃, and the PH value is less than or equal to 6; the flame retardant APP has the model number of APP-451, the polymerization degree is more than or equal to 1000, the flame retardant APP is white powder, the average particle size is less than or equal to 20 mu m, the phosphorus content is more than or equal to 30 percent, the nitrogen content is more than or equal to 13 percent, and the thermal decomposition temperature is more than or equal to 275 ℃.
The flame-retardant synergist adopted by the invention is graphene, and the single-layer rate of the flame-retardant synergist is more than or equal to 60%. The preferable flame retardant synergist is lipophilic graphene powder, the number of layers/thickness of the flame retardant synergist is 1-3, the single-layer rate is more than 80%, the carbon content is more than or equal to 98%, the sheet diameter (D50) is 4-7 mu m, the sheet diameter (D90) is 9-11 mu m, the average diameter-thickness ratio is 8500, the flame retardant synergist is black-gray powder, and the bulk density is 0.01-0.02 g/ml.
The dispersant adopted by the invention is a sodium polyacrylate anionic dispersant, the trademark of which is PL30 produced by Craine corporation, the content of active substances is 30 percent, and the appearance of the product is colorless to light yellow liquid.
The lubricant adopted by the invention is E wax, the appearance of the lubricant is yellowish powder, the acid value is 17mgKOH/g, and the density is 1.00-1.03g/cm3The saponification value was 145 mgKON/g.
The antioxidant adopted by the invention is hindered phenol antioxidant such as 1010, 1076, 1098 and the like. The preferable antioxidant is the antioxidant 1010 produced by German Pasteur company, the appearance of the antioxidant is white crystal powder, the effective component is more than or equal to 99 percent, the melting point is 110-125 ℃, the volatile matter is less than or equal to 0.5 percent, and the gray scale is less than or equal to 0.1 percent. The length-diameter ratio (L/D) of the double-screw extruder is 35-52. A twin screw extruder is preferred which has an L/D of 42.
The following examples further illustrate the present invention but are not to be construed as limiting the invention. Modifications or substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit and scope of the invention. The experimental methods and reagents of the formulations not specified in the examples are in accordance with the conventional conditions in the art.
The raw material grades and physical properties used in the following examples and comparative examples of the present invention are shown in table 1:
TABLE 1
Figure BDA0002338380920000031
Figure BDA0002338380920000041
In the following examples and comparative examples, a graphene synergistic flame retardant ABS/SBS composite material was prepared, the hardness of which was measured using a Rockwell hardness tester (R Table), and the hardness value was read at 1 second press. The mechanical property is tested on a universal electronic tensile machine according to the GB/T2951.11-2008 standard, and the tensile speed is 100 mm/min; the IZOD notched impact strength of the alloy is measured at room temperature of 23 ℃ and at a low temperature of-40 ℃ respectively, and the unit is KJ/m2. The flame retardance is respectively expressed by UL94 vertical burning grade, peak heat release rate (PHHR) and Limiting Oxygen Index (LOI), and the UL94 vertical burning sample bar size: the length/width/thickness is 125mm/12.5mm/(0.8mm/1.6mm/3.0 mm); the peak value of the heat release rate IS tested by a cone calorimeter according to the experiment standard of IS 05660-1, the specification of the flame-retardant sample IS 10cm multiplied by 3mm, and the radiation heat flow intensity IS 35kW/m2(ii) a Spline size of LOI: the length/width/thickness was 125mm/12.5mm/3.0 mm. The method for testing the precipitation resistance comprises the following steps: the sample is placed in an oven with the humidity of 80 ℃/80 ℃ for 7 days continuously, then is taken out and cooled to the room temperature, and the surface of the material is observed whether the precipitation phenomenon exists or not.
The examples and comparative examples described below, which test the samples used, were injection molded at 260 ℃.
The formulations of examples 1 to 4 of the present invention and comparative examples 5 to 10 are shown in Table 2:
TABLE 2
Figure BDA0002338380920000042
Figure BDA0002338380920000051
The test results and performance indexes of examples 1 to 4 and comparative examples 5 to 10 of the present invention are shown in table 3:
TABLE 3
Figure BDA0002338380920000052
As shown in Table 3, in examples 1 to 4, the binary blend of ABS and SBS was used as the base material, and SBS-g-NH was added2As a compatibilizer, a flame-retardant system consisting of polyphosphate flame retardants (MPP and APP) and graphene powder is adopted, and a polyacrylate anionic dispersing agent is added to prepare the graphene synergistic flame-retardant ABS/SBS composite material. As can be seen from the test results of examples 1-2 in Table 3: the prepared flame-retardant ABS/SBS composite material has UL94 vertical burning (thickness 1.6mm) reaching V-0 level, LOI not less than 28.3%, and heat release rate peak value not more than 350KW/m2No precipitation at constant temperature and constant humidity, and IZOD notch impact strength (23 ℃) of more than or equal to 25.1KJ/m2IZOD notched impact strength (-40 ℃) of not less than 19.1KJ/m2(ii) a Examples 3 to 4: UL94 vertical burning (thickness 0.8mm) reaches V-0 level, LOI is more than or equal to 32.5%, peak value of heat release rate is less than or equal to 237KW/m2No precipitation at constant temperature and constant humidity, and IZOD notch impact strength (23 ℃) of more than or equal to 22.3KJ/m2IZOD notched impact strength (-40 ℃) of not less than 17.3KJ/m2(ii) a The flame retardance and the toughness of the flame-retardant polyurethane are obviously improved, no micromolecules are separated out, and the flame-retardant polyurethane has good comprehensive performance.
The results of the tests of comparative examples 5 to 6 (with TPP and RDP added) in Table 3 show that: prepared flame-retardant ABSThe UL94 vertical combustion of the/SBS composite material is only FAIL (thickness 1.6mm) and V-1 grade (thickness 3.0mm), and the obvious precipitation phenomenon occurs in the constant temperature and humidity test; comparative examples 7 to 9 (without addition of graphene KNG-G2-2 or dispersant PL30) in which UL94 vertical burning (thickness 1.6mm) was only V-1 or V-2 grade; comparative example 10 (without SBS-P2000) had an IZOD notched impact strength of only 14.8KJ/m2(23℃)、5.3KJ/m2(-40℃)。
The embodiment shows that the graphene synergistic flame-retardant ABS/SBS composite material prepared by the invention has the characteristics of good flame retardance, no precipitation, high toughness and low temperature resistance.
While specific embodiments of the invention have been disclosed, the invention is not limited thereto, and any local variations in the formulations and processes based thereon are intended to be within the scope of the invention.

Claims (10)

1. The graphene synergistic flame-retardant ABS/SBS composite material is characterized in that: the raw materials comprise the following components in parts by weight: 100 parts of ABS resin, 8-100 parts of toughening agent SBS and compatibilizer SBS-g-NH20.5-15 parts of a flame retardant, 10-60 parts of a flame retardant synergist, 2-8 parts of a flame retardant synergist, 0.2-2 parts of a dispersant, 0.1-3 parts of a lubricant and 0.1-2 parts of an antioxidant.
2. The composite material of claim 1, wherein: the melt index of the ABS resin is more than or equal to 15g/10min (220 ℃/10kg), and the specific gravity of the ABS resin is 1.05g/cm3Tensile strength is more than or equal to 40MPa, and IZOD (23 ℃) notch impact strength is more than or equal to 20KJ/m2The IZOD (-40 ℃) notch impact strength is more than or equal to 8.5KJ/m2。
3. The composite material of claim 1, wherein: the compatibilizer SBS-g-NH2，NH2The grafting ratio of (A) is 0.1-2.5%.
4. The composite material of claim 1, wherein: the flame retardant is polyphosphate or phosphate flame retardant selected from melamine polyphosphate MPP, ammonium polyphosphate APP, triphenyl phosphate TPP or resorcinol bis (diphenyl phosphate) RDP.
5. The composite material of claim 1, wherein: the flame-retardant synergist is graphene, and the single-layer rate of the flame-retardant synergist is more than or equal to 60%.
6. The composite material of claim 1, wherein: the dispersant is sodium polyacrylate anionic dispersant.
7. The composite material of claim 1, wherein: the lubricant is E wax.
8. The composite material of claim 1, wherein: the antioxidant is hindered phenol antioxidant selected from antioxidant 1010, antioxidant 1076 or antioxidant 1098.
9. The preparation method of the graphene synergistic flame-retardant ABS/SBS composite material as claimed in claim 1, is characterized in that: ABS resin, a toughening agent SBS and a compatibilizer SBS-g-NH2The flame retardant, the flame-retardant synergist, the dispersing agent, the lubricant and the antioxidant are sequentially added into a high-speed mixer, fully mixed for 5-6 min, and then subjected to melt extrusion granulation at 230-280 ℃ through a double-screw extruder to obtain the composite material.
10. The method of claim 9, wherein: the length-diameter ratio (L/D) of the double-screw extruder is 35-52.
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Cited By (1)

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CN114213759A (en) * 2022-01-04 2022-03-22 深圳中塑化工高性能材料有限公司 Preparation method and application of polyphosphate grafted graphene flame-retardant modified polypropylene

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CN103804845A (en) * 2014-01-28 2014-05-21 盐城纳新天地新材料科技有限公司 High-strength high thermal conductivity ABS master batch and preparation method thereof
CN104371265A (en) * 2014-12-11 2015-02-25 东莞市国立科技有限公司 Reclaimed ABS (acrylonitrile butadiene styrene) environment-friendly modified material and preparation method thereof

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EP1777262A1 (en) * 2005-10-24 2007-04-25 Basf Aktiengesellschaft Carbon nanotubes reinforced thermoplastic molding compositions and production process therefor
CN103804845A (en) * 2014-01-28 2014-05-21 盐城纳新天地新材料科技有限公司 High-strength high thermal conductivity ABS master batch and preparation method thereof
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Publication number Priority date Publication date Assignee Title
CN114213759A (en) * 2022-01-04 2022-03-22 深圳中塑化工高性能材料有限公司 Preparation method and application of polyphosphate grafted graphene flame-retardant modified polypropylene
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