CN112457623B - High-impact-resistance and yellowing-resistance flame-retardant ABS material and preparation method thereof - Google Patents
High-impact-resistance and yellowing-resistance flame-retardant ABS material and preparation method thereof Download PDFInfo
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- 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
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Abstract
The invention relates to a high-impact-resistance and yellowing-resistance flame-retardant ABS material and a preparation method thereof, and the material specifically comprises the following raw materials in parts by weight: 45-70 parts of ABS resin, 10-30 parts of an organic halide flame retardant, 2-8 parts of a compound anti-yellowing stabilizer and 1-3 parts of a weather-resistant auxiliary agent, wherein the compound anti-yellowing stabilizer is prepared by mixing a stearic acid metal salt and layered nano montmorillonite according to a blending ratio of 5:1 by an intercalation compounding method; the invention has the advantages that: aiming at the inherent problems that the impact toughness of the traditional flame-retardant ABS material is greatly reduced after a flame retardant is added and the flame retardant property of the ABS is lost after the rubber elastomer is toughened, chlorinated polyethylene with double special effects of toughening and flame retardance is used as a flame-retardant synergistic additive, and aiming at the performance defects that chlorinated polyethylene CPE is easy to process and discolor and degrade in a high-temperature and high-humidity environment, a high-efficiency compound type yellowing-resistant stabilizer is added, so that the multiple characteristics of high impact resistance, yellowing resistance and excellent processing stability of the flame-retardant ABS material are realized.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a flame-retardant ABS material with high impact resistance and yellowing resistance and a preparation method thereof.
Background
The ABS material is a ternary alloy blending material consisting of styrene, butadiene and acrylonitrile, different structural components endow the ABS material with different characteristics, wherein the styrene can improve the processing fluidity of the material, the butadiene is one of the components of the rubber material and can improve the impact toughness of the ABS material, particularly the stress cracking resistance in a low-temperature environment, and the acrylonitrile endows the ABS material with good chemical resistance, environmental stability and certain flame retardant property. Due to the excellent comprehensive characteristics of ABS materials, ABS materials are widely applied to the fields of current automobiles, industrial electronics, household appliances, communication equipment and the like.
When the ABS is applied to the field of industrial electronic and electrical appliances, the ABS is usually used as a molding material of shell parts, and the parts often require extremely high comprehensive performance due to the particularity of the use environment, such as high flame retardance of UL 94V-0 grade, excellent notch impact toughness, good processing fluidity and long-term stability under a melting condition, and the like, so that higher-level requirements are provided for modification of the ABS material, and the traditional modification technical scheme can only meet one of the requirements. CN111500011A describes a flame-retardant weather-resistant ABS material, which adopts a bromine-antimony composite flame-retardant system to realize the obvious improvement of the flame-retardant performance of the material, but has no targeted improvement on the notch impact of the material, especially the impact toughness in a low-temperature environment; CN108219351B focuses on the improvement of high impact property of flame-retardant ABS, but the addition of large amount of elastomer inevitably affects the improvement of flame-retardant property of ABS. Therefore, how to synergistically improve the flame retardancy, the impact resistance and the environmental stability of ABS becomes a technical problem to be solved urgently.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a flame-retardant ABS material with high impact resistance and yellowing resistance.
The purpose of the invention is realized by the following technical scheme: a flame-retardant ABS material with high impact resistance and yellowing resistance is characterized in that: the feed comprises the following raw materials in parts by weight:
the compound anti-yellowing stabilizer is prepared by mixing metal stearate and layered nano montmorillonite in a blending ratio of 3:1 by an intercalation compounding method.
Furthermore, the styrene-butadiene-Acrylonitrile (ABS) resin is prepared by a bulk method, the melt index of the styrene-butadiene-Acrylonitrile (ABS) resin is 8-30 g/10min under the test conditions of 220 ℃ and 10Kg, and the butadiene content is less than or equal to 18%.
Further, the organic halide flame retardant is one or more of decabromodiphenylethane, tribromophenyl triazine, halogenated epoxy resin and chlorinated polyethylene.
Furthermore, the weather-resistant auxiliary agent is a complex ligand of a phosphite antioxidant and a hindered phenol antioxidant.
Further, the preparation method of the compound type anti-yellowing stabilizer comprises the following steps: weighing 5 parts of metal stearate, preparing the metal stearate and deionized water into a water dispersion solution with the concentration of 1: 10-1: 50, and adding a nanoscale lamellar montmorillonite carrier under the action of an ultrasonic dispersion machine, wherein the ultrasonic power is 52w, and the frequency is 55 Hz; raising the temperature to 80 ℃, ultrasonically stirring for 30min to ensure that a lamellar structure of the montmorillonite is fully opened, metal stearate auxiliary agent molecules are fully diffused into an intercalation structure of the nano montmorillonite, and then removing water contained in the nano montmorillonite through repeated rotary evaporation treatment, thereby obtaining the compound anti-yellowing stabilizer.
Further, the metal stearate is one or more of calcium stearate, barium stearate, magnesium stearate, zinc stearate and rare earth stearate.
Furthermore, the nano-montmorillonite is a layered aluminum magnesium silicate clay mineral with the structural layer thickness reaching the nano-scale size, the parallel wafer row thickness is less than or equal to 20 nanometers, and the montmorillonite content is more than or equal to 99.5 percent.
The second purpose of the invention is to provide a preparation method of a flame-retardant ABS material with high impact resistance and yellowing resistance, which is characterized by comprising the following steps:
(1) weighing ABS resin, organic halide flame retardant, compound yellowing-resistant stabilizer and weather-resistant auxiliary agent according to the weight percentage, and uniformly mixing to obtain the mixed raw material.
(2) Drying the mixed raw materials, placing the dried mixed raw materials into a main feeding bin of a meshing co-rotating double-screw extruder, adding the dried mixed raw materials into a machine barrel of the extruder through a feeding screw, and setting the temperature as follows: the flame retardant ABS material with high impact resistance and yellowing resistance is prepared by melt extrusion, cooling, granulation and drying at the temperature of 120 ℃, 170 ℃, 180 ℃, 190 ℃, 195 ℃, 190 ℃ and the rotation speed of a main engine of 250 r/min.
Compared with the prior art, the invention has the following beneficial effects:
(1) based on the technical problems of 'flame retardance, impact resistance, stability' and the like inherent in the conventional scheme of flame-retardant ABS, the high-efficiency bromide flame retardant and the high-impact-resistance low-cost chlorinated polyethylene are taken as a compound flame retardant system, and the ABS material is ensured to achieve high flame-retardant property by sufficient halogen content.
(2) The chlorinated polyethylene CPE can improve the flame retardance of the material and obviously improve the normal-temperature and low-temperature notch impact toughness of the ABS material, which is a characteristic that the traditional rubber elastomer does not have for toughening; meanwhile, aiming at the defects that CPE is not durably processed and is easy to be thermally decomposed and yellowed, the high-efficiency compound yellowing-resistant stabilizer is adopted, the stability problem of CPE is well solved, and good processing stability is provided for the flame-retardant ABS material.
(3) The flame-retardant ABS blending material with high impact resistance and yellowing resistance prepared by the technical scheme of the invention has good impact toughness performance in both a conventional environment (23 ℃) and a low-temperature environment (30 ℃), especially the multiaxial instrument impact in the low-temperature environment, the absorbed impact energy can be kept above 25J, the fracture mode is toughness fracture, and the modification effect which cannot be achieved by the traditional elastomer toughening mode in the same environment is achieved; UL94 vertical burning tests show that the flame retardant grade of the modified ABS material can reach the highest UL945VA (3.2mm), the stability of the material under a melting condition can be obviously improved by adding the yellowing-resistant stabilizer, and even if the residence time in an injection molding machine exceeds 10min, the color difference value delta E of an injection molding sample is still kept within 0.5, and the excellent yellowing-resistant stability is shown.
Detailed Description
The invention is further illustrated by the following specific examples, which are intended to be illustrative only and not limiting.
The raw materials used in the embodiment of the invention are as follows:
ABS: ABS-3513 is prepared by a bulk method, wherein the melt index MFR is 8g/10min (220 ℃, 10Kg), and the butadiene content is 17 percent.
Organic halide flame retardant-1: decabromodiphenylethane HT-106, white powder, Shandong Jinnan Taxing Fine chemical Co., Ltd., effective bromine content is not less than 82%.
Organic halide flame retardant-2: bromotriazine FR-245, white powder, Shandong Asahi Shaoxing Co., Ltd., available bromine content not less than 67%.
Organic halide flame retardant-3: chlorinated polyethylene CPE-132, white powder, available chlorine content 32 + -1% from Hangzhou Koli chemical industries, Ltd.
Stearic acid metal salt-1: calcium stearate Cast, white powder, Hebei Shijiazhuang Yongfeng chemical plastic additive factory, free acid content less than or equal to 0.5%.
Stearic acid metal salt-2: WWP-C of stearic acid rare earth salt, white or yellowish powder, Guangdong Weilinnan new materials science and technology company, and the content of free acid is less than or equal to 0.2 percent.
Nano montmorillonite: DK2 nanometer organic montmorillonite, white or off-white fine powder, Zhejiang Fenghong New Material GmbH, XRD 001:2.4nm, wafer layer thickness less than or equal to 25nm, montmorillonite content greater than or equal to 95%.
Weather-resistant auxiliary agent: phosphite 626/hindered amine stabilizer 944 was prepared as a 1:2, mixing and using the mixture according to the proportion of 2, and self-making.
And (3) product performance testing:
impact properties: the method is carried out on a simple beam impact tester according to the ISO179-1 standard, the notch of the sample strip is A type, and the test is carried out under the conditions of normal temperature (23 ℃), low temperature (-10 ℃) and extremely low temperature (-40 ℃) respectively.
Low temperature instrument impact performance: the method is carried out according to ISO6603-2 standard, the testing temperature is-40 ℃, the testing speed is 2mm/s penetration energy is 55J, and the fracture type of the material is judged to be brittle fracture or ductile fracture according to the notch type and the energy absorption condition generated after the impact of a standard sample strip.
Flame retardant property: according to the standard test method of UL94 vertical burning, the test is carried out in a Delik DRK-310 horizontal vertical burning tester, and the test sample strips are 1.6mm and 3.2mm respectively.
Yellowing resistance test: the method is carried out according to a standard method special for SAE J2527 automobile exterior parts, a standard sample plate with the size of 100 multiplied by 10 multiplied by 3.2mm is injected, the initial color difference value of the surface of the sample plate is tested, then an ATLAS Ci4000 xenon lamp aging tester is placed, the testing period is 500h, and the surface gloss of the sample plate is tested after the test is completed; and testing the surface color difference of the sample plate by using a standard color difference meter, comparing the surface color difference with an initial value, and calculating to obtain the color difference value delta E of the sample plate.
Example 1
Weighing ABS resin, organic halide flame retardant, compound anti-yellowing stabilizer and weather-resistant auxiliary agent according to the weight percentage of the example 1 in the table 1, and uniformly mixing to obtain a mixed raw material.
Drying the mixed raw materials, placing the dried mixed raw materials into a main feeding bin of a meshing co-rotating double-screw extruder, adding the dried mixed raw materials into a machine barrel of the extruder through a feeding screw, and setting the temperature as follows: the flame retardant ABS material with high impact resistance and yellowing resistance is prepared by melt extrusion, cooling, granulation and drying at the temperature of 120 ℃, 170 ℃, 180 ℃, 190 ℃, 195 ℃, 190 ℃ and the rotation speed of a main engine of 250 r/min.
Example 2
Weighing ABS resin, organic halide flame retardant, compound yellowing-resistant stabilizer and weather-resistant auxiliary agent according to the weight percentage of the example 2 in the table 1, and uniformly mixing to obtain a mixed raw material.
Drying the mixed raw materials, placing the dried mixed raw materials into a main feeding bin of a meshing co-rotating double-screw extruder, adding the dried mixed raw materials into a machine barrel of the extruder through a feeding screw, and setting the temperature as follows: the flame retardant ABS material with high impact resistance and yellowing resistance is prepared by melt extrusion, cooling, granulation and drying at the temperature of 120 ℃, 170 ℃, 180 ℃, 190 ℃, 195 ℃, 190 ℃ and the rotation speed of a main engine of 250 r/min.
TABLE 1 formulation of high impact, yellowing resistant flame retardant ABS materials (unit: gram)
Example 3
Weighing ABS resin, organic halide flame retardant, compound anti-yellowing stabilizer and weather-resistant auxiliary agent according to the weight percentage of the embodiment 3 in the table 1, and uniformly mixing to obtain a mixed raw material.
Drying the mixed raw materials, placing the dried mixed raw materials into a main feeding bin of a meshing co-rotating double-screw extruder, adding the dried mixed raw materials into a machine barrel of the extruder through a feeding screw, and setting the temperature as follows: the flame retardant ABS material with high impact resistance and yellowing resistance is prepared by melt extrusion, cooling, granulation and drying at the temperature of 120 ℃, 170 ℃, 180 ℃, 190 ℃, 195 ℃, 190 ℃ and the rotation speed of a main engine of 250 r/min.
Example 4
Weighing ABS resin, organic halide flame retardant, compound yellowing-resistant stabilizer and weather-resistant auxiliary agent according to the weight percentage of the example 4 in the table 1, and uniformly mixing to obtain a mixed raw material.
Drying the mixed raw materials, placing the dried mixed raw materials into a main feeding bin of a meshing co-rotating double-screw extruder, adding the dried mixed raw materials into a machine barrel of the extruder through a feeding screw, and setting the temperature as follows: the flame retardant ABS material with high impact resistance and yellowing resistance is prepared by melt extrusion, cooling, granulation and drying at the temperature of 120 ℃, 170 ℃, 180 ℃, 190 ℃, 195 ℃, 190 ℃ and the rotation speed of a main engine of 250 r/min.
Example 5
Weighing ABS resin, organic halide flame retardant, compound yellowing-resistant stabilizer and weather-resistant auxiliary agent according to the weight percentage of the example 5 in the table 1, and uniformly mixing to obtain a mixed raw material.
Drying the mixed raw materials, placing the dried mixed raw materials into a main feeding bin of a meshing co-rotating double-screw extruder, adding the dried mixed raw materials into a machine barrel of the extruder through a feeding screw, and setting the temperature as follows: the flame retardant ABS material with high impact resistance and yellowing resistance is prepared by melt extrusion, cooling, granulation and drying at the temperature of 120 ℃, 170 ℃, 180 ℃, 190 ℃, 195 ℃, 190 ℃ and the rotation speed of a main engine of 250 r/min.
Example 6
Weighing ABS resin, organic halide flame retardant, compound yellowing-resistant stabilizer and weather-resistant auxiliary agent according to the weight percentage of the example 6 in the table 1, and uniformly mixing to obtain a mixed raw material.
Drying the mixed raw materials, placing the dried mixed raw materials into a main feeding bin of a meshing co-rotating double-screw extruder, adding the dried mixed raw materials into a machine barrel of the extruder through a feeding screw, and setting the temperature as follows: the flame retardant ABS material with high impact resistance and yellowing resistance is prepared by melt extrusion, cooling, granulation and drying at the temperature of 120 ℃, 170 ℃, 180 ℃, 190 ℃, 195 ℃, 190 ℃ and 190 ℃ at the host rotation speed of 250 r/min.
Comparative example 1
Weighing ABS resin, organic halide flame retardant and weather-resistant auxiliary agent according to the weight percentage of the comparative example 1 in the table 1, and uniformly mixing to obtain the mixed raw material.
Drying the mixed raw materials, placing the dried mixed raw materials into a main feeding bin of a meshing co-rotating double-screw extruder, adding the dried mixed raw materials into a machine barrel of the extruder through a feeding screw, and setting the temperature as follows: 120 ℃, 170 ℃, 180 ℃, 190 ℃, 195 ℃, 190 ℃ and the rotating speed of a main engine is 250 revolutions per minute, and the flame-retardant ABS material is prepared by melt extrusion, cooling, granulation and drying treatment
TABLE 2 test results of high impact, yellowing resistant flame retardant ABS materials
From the material property test data of each of examples 1 to 6 and comparative example 1 in Table 2, the conventional flame retardant was added to the flame retardant ABS material (Examples 1, 2) had a very large negative effect on the chipping resistance of the material, and the chipping impact resin at normal and low temperatures was only 10kJ/m 2 The addition of chlorinated polyethylene CPE can effectively compensate for the above-mentioned toughness loss, but since the CPE itself has a low halogen content, the flame retardancy of ABS is effectively improved (example 3), and the flame retardancy of ABS needs to be improved to UL945VA (3.2mm) to the maximum by using the CPE in combination with a high-efficiency brominated organic flame retardant.
Further comparing examples 3-5, it is known that the use of chlorinated polyethylene CPE can achieve the purpose of toughening ABS, but the defects of poor chemical stability and easy processing yellowing are exposed. When the efficient and yellowing-resistant compound stabilizer is optimally used, the yellowing value delta E of the flame-retardant ABS can be effectively controlled to be at least 0.25 (example 6), and the flame retardance, the normal-temperature resistance and the low-temperature resistance of the material reach ideal balance points.
The high-impact-resistance and yellowing-resistance flame-retardant ABS blending material provided by the invention can be widely applied to the fields of current hot materials such as charging pile shells of new energy automobiles, household appliance shells, industrial electronic and electric appliance elements and the like, and the excellent yellowing resistance of the blending material is particularly suitable for shell materials and functional parts which have complex structural design, long processing and flowing process and long retention time in an injection molding machine, so that extremely favorable basic conditions can be created for the wide application of the materials in the related fields.
Claims (5)
1. A flame-retardant ABS material with high impact resistance and yellowing resistance is characterized in that: the feed comprises the following raw materials in parts by weight:
45-70 parts of ABS resin;
10 to 30 parts of an organic halide flame retardant;
2-8 parts of a compound anti-yellowing stabilizer;
1-3 parts of a weather-resistant auxiliary agent;
wherein the compound anti-yellowing stabilizer is prepared by mixing metal stearate and layered nano montmorillonite in a blending ratio of 3:1 by an intercalation compounding method;
the metal stearate is one or more of calcium stearate, barium stearate, magnesium stearate, zinc stearate and rare earth stearate;
the nano-montmorillonite is a layered aluminum-magnesium silicate clay mineral with the structural layer thickness reaching the nanoscale size, the thickness of the parallel wafer rows is less than or equal to 20 nanometers, and the montmorillonite content is more than or equal to 99.5 percent;
the preparation method of the compound anti-yellowing stabilizer comprises the following steps: weighing 5 parts of metal stearate, preparing the metal stearate and deionized water into a water dispersion solution with the concentration of 1: 10-1: 50, and adding a nanoscale lamellar montmorillonite carrier under the action of an ultrasonic dispersion machine, wherein the ultrasonic power is 52w, and the frequency is 55 Hz; raising the temperature to 80 ℃, ultrasonically stirring for 30min to ensure that a lamellar structure of the montmorillonite is fully opened, metal stearate auxiliary agent molecules are fully diffused into an intercalation structure of the nano montmorillonite, and then removing water contained in the nano montmorillonite through repeated rotary evaporation treatment, thereby obtaining the compound anti-yellowing stabilizer.
2. The high impact resistant, yellowing resistant flame retardant ABS material of claim 1 wherein: the ABS resin is prepared by a bulk method, and under the test conditions of 220 ℃ and 10Kg, the melt index of the ABS resin is 8-30 g/10min, and the butadiene content is less than or equal to 18%.
3. The high impact resistant, yellowing resistant flame retardant ABS material of claim 1 wherein: the organic halide flame retardant is one or more of decabromodiphenylethane, tribromophenyl triazine, halogenated epoxy resin and chlorinated polyethylene.
4. The high impact resistant, yellowing resistant flame retardant ABS material of claim 1 wherein: the weather-resistant auxiliary agent is a complex ligand of a phosphite antioxidant and a hindered phenol antioxidant.
5. The preparation method of the high impact resistance and yellowing resistance flame retardant ABS material of claim 1 is characterized by comprising the following steps:
(1) weighing ABS resin, organic halide flame retardant, compound anti-yellowing stabilizer and weather-resistant auxiliary agent according to the weight percentage, and uniformly mixing to obtain a mixed raw material;
45-70 parts of ABS resin;
10 to 20 parts of an organic halide flame retardant;
2-8 parts of a compound type yellowing-resistant stabilizer;
1-3 parts of a weather-resistant auxiliary agent;
(2) drying the mixed raw materials, placing the dried mixed raw materials into a main feeding bin of a meshing co-rotating double-screw extruder, adding the dried mixed raw materials into a machine barrel of the extruder through a feeding screw, and setting the temperature as follows: the flame retardant ABS material with high impact resistance and yellowing resistance is prepared by melt extrusion, cooling, granulation and drying at the temperature of 120 ℃, 170 ℃, 180 ℃, 190 ℃, 195 ℃, 190 ℃ and 190 ℃ at the host rotation speed of 250 r/min.
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