CN118027575A - Heat-resistant flame-retardant microporous expanded polystyrene material and preparation method thereof - Google Patents
Heat-resistant flame-retardant microporous expanded polystyrene material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 127
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000003063 flame retardant Substances 0.000 title claims abstract description 40
- 239000004794 expanded polystyrene Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000004793 Polystyrene Substances 0.000 claims abstract description 73
- 229920002223 polystyrene Polymers 0.000 claims abstract description 73
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 20
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
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- 239000002077 nanosphere Substances 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 10
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 239000003607 modifier Substances 0.000 claims description 10
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 10
- 239000004156 Azodicarbonamide Substances 0.000 claims description 9
- XOZUGNYVDXMRKW-AATRIKPKSA-N azodicarbonamide Chemical compound NC(=O)\N=N\C(N)=O XOZUGNYVDXMRKW-AATRIKPKSA-N 0.000 claims description 9
- 235000019399 azodicarbonamide Nutrition 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- 238000000967 suction filtration Methods 0.000 claims description 7
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 6
- 238000001125 extrusion Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 229920000877 Melamine resin Polymers 0.000 claims description 5
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 5
- AGXUVMPSUKZYDT-UHFFFAOYSA-L barium(2+);octadecanoate Chemical compound [Ba+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AGXUVMPSUKZYDT-UHFFFAOYSA-L 0.000 claims description 5
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 5
- 239000008116 calcium stearate Substances 0.000 claims description 5
- 235000013539 calcium stearate Nutrition 0.000 claims description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 5
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 5
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 5
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 4
- 239000004698 Polyethylene Substances 0.000 claims description 4
- -1 polyethylene Polymers 0.000 claims description 4
- 229920000573 polyethylene Polymers 0.000 claims description 4
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 3
- 239000004209 oxidized polyethylene wax Substances 0.000 claims description 3
- 235000013873 oxidized polyethylene wax Nutrition 0.000 claims description 3
- ZDWQSEWVPQWLFV-UHFFFAOYSA-N C(CC)[Si](OC)(OC)OC.[O] Chemical compound C(CC)[Si](OC)(OC)OC.[O] ZDWQSEWVPQWLFV-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 1
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 238000000354 decomposition reaction Methods 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
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- 238000012986 modification Methods 0.000 description 1
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- 239000012299 nitrogen atmosphere Substances 0.000 description 1
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- 238000001757 thermogravimetry curve Methods 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
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- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the technical field of high polymer materials, in particular to a heat-resistant flame-retardant microporous expanded polystyrene material and a preparation method thereof; the heat-resistant flame-retardant microporous expanded polystyrene material is prepared from the following raw materials in parts by weight: 50 to 60 parts of polystyrene, 8 to 12 parts of functional auxiliary agents, 10 to 12 parts of synergistic auxiliary agents, 6 to 10 parts of composite foaming agents, 6 to 10 parts of lubricants and 3 to 5 parts of antioxidants; the polystyrene material prepared by the invention is prepared by weighing polystyrene, functional auxiliary agent, synergistic auxiliary agent, composite foaming agent, lubricant and antioxidant, mixing in mixing equipment, heating in an extruder, and then melting, mixing, foaming and extruding to obtain a heat-resistant flame-retardant microporous foamed polystyrene material finished product; the polystyrene material prepared by the invention not only has excellent heat resistance, but also has excellent flame retardant property; and the foam cell density is high, the foam cell size is small, and the foaming effect is good.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a heat-resistant flame-retardant microporous expanded polystyrene material and a preparation method thereof.
Background
Polystyrene has the characteristics of hard quality, good transparency, rigidity, electrical insulation, low hygroscopicity, low price, easy dyeing, easy processing, no change of heat conductivity with temperature and the like, and has wide application in various fields of industry and civilian use, so that the polystyrene becomes one of four general plastics at present.
The traditional polystyrene foaming composite material is basically prepared by using the general polystyrene matched with a foaming agent, but the glass transition temperature of the general polystyrene is low, the high temperature resistance is poor, marks are easily left on the surface when the polystyrene foaming composite material is contacted with a high-temperature medium of more than 100 ℃, the performance of the polystyrene foaming composite material is influenced, and meanwhile, the traditional polystyrene foaming composite material also lacks excellent flame retardant performance.
Accordingly, the present invention provides a heat-resistant flame-retardant microporous expanded polystyrene material and a preparation method thereof, which are used for solving the above-mentioned related technical problems.
Disclosure of Invention
The invention aims to provide a heat-resistant flame-retardant microporous expanded polystyrene material and a preparation method thereof, and the prepared polystyrene material has excellent heat resistance and flame retardance; and has high cell density, small cell size (diameter) and good foaming effect.
In order to achieve the above purpose, the present invention provides the following technical solutions:
The first aspect of the invention: the heat-resistant flame-retardant microporous expanded polystyrene material is prepared from the following raw materials in parts by weight: 50 to 60 parts of polystyrene, 8 to 12 parts of functional auxiliary agents, 10 to 12 parts of synergistic auxiliary agents, 6 to 10 parts of composite foaming agents, 6 to 10 parts of lubricants and 3 to 5 parts of antioxidants.
The invention is further provided with: the preparation process of the functional auxiliary agent comprises the following steps:
Placing a proper amount of carbon nanospheres into a proper amount of hydrochloric acid with the mass concentration of 35% according to the solid-to-liquid ratio of 0.02-0.05 g/mL, and treating for 240-250 min under the conditions of 60-70 r/min and 60-64 ℃; cooling to room temperature, filtering, washing the obtained product with deionized water for 2-6 times, and treating the obtained washed product in an oven at 85-95 ℃ for 40-50 min to obtain a first material;
Placing a proper amount of modifier into a proper amount of deionized water according to a solid-to-liquid ratio of 0.018-0.024 g/mL, mixing for 20-30 min, adding a proper amount of hydrochloric acid solution into the mixture, and adjusting the pH of the mixture to 6.2-6.5 to obtain a modified solution;
dispersing a proper amount of silicon nitride in a proper amount of modified solution according to a solid-liquid ratio of 0.12-0.22 g/mL, mixing for 20-30 min, then treating for 120-140 min at 40-42 ℃, and treating for 100-120 min in an oven at 65-75 ℃ after suction filtration to obtain a second material;
Dispersing a proper amount of the first material in a proper amount of deionized water according to a solid-liquid ratio of 0.24-0.28 g/mL, mixing for 30-40 min, adding a second material into the obtained first material solution, treating for 10-15 min under the condition of 340-540 r/min, treating for 300-320 min under the condition of 100-110 ℃, filtering, washing for 3-5 times with deionized water, and treating for 120-140 min in an oven at 80-90 ℃ to obtain the functional auxiliary agent.
The invention is further provided with: the modifier is any one of 3-aminopropyl trimethoxy silane, gamma-aminopropyl trimethoxy silane and 3-glycidol ether oxygen propyl trimethoxy silane.
The invention is further provided with: the addition amount of the second material is 2.5-4.5% of the mass of the first material solution.
The invention is further provided with: the preparation process of the synergistic auxiliary agent comprises the following steps:
placing a proper amount of melamine into a proper amount of glycol according to a solid-to-liquid ratio of 0.036-0.056 g/mL, and mixing for 30-40 min under the conditions of 70-80 ℃ and 220-320 r/min to obtain a first mixed solution;
placing a proper amount of beta- (N-phenylformamide) ethyl methyl aluminum phosphinate into a proper amount of first mixed solution according to a solid-to-liquid ratio of 0.012-0.036 g/mL, and mixing for 10-15 min at a temperature of 85-90 ℃ under a condition of 540-640 r/min to obtain a second mixed solution;
Adding phosphoric acid into the obtained second mixed solution, mixing for 180-200 min at the temperature of 75 ℃ under the condition of 180-280 r/min, cooling to room temperature after mixing, centrifuging for 4-6 min under the condition of 8000-12000 r/min, washing the obtained centrifugal product with absolute ethyl alcohol for 2-8 times, and then treating in an oven at the temperature of 60-65 ℃ for 20-26 h to obtain the synergistic auxiliary agent.
The invention is further provided with: the adding amount of the phosphoric acid is 2.6-4.2% of the mass of the second mixed solution.
The invention is further provided with: the composite foaming agent is prepared from azodicarbonamide and stearate in a mass ratio of 0.3-0.6: 1 are mixed and compounded.
The invention is further provided with: the stearate is prepared from zinc stearate, calcium stearate and barium stearate according to the mass ratio of 0.3-0.7: 0.2 to 0.4:1 are mixed and compounded.
The invention is further provided with: the lubricant is selected from any one of polyethylene wax and oxidized polyethylene wax.
The invention is further provided with: the antioxidant is selected from any one of antioxidant 1010 and antioxidant 168.
The second aspect of the invention: the preparation process of heat-resisting flame-retarding microporous foamed polystyrene material includes the following steps:
Firstly, accurately weighing polystyrene, functional auxiliary agent, synergistic auxiliary agent, composite foaming agent, lubricant and antioxidant respectively, and then placing the materials in mixing equipment to mix for 20-30 min at 170-200 ℃ to obtain a mixed material;
and step two, placing the obtained mixture into an extruder, heating to 200-220 ℃, and then performing melt mixing foaming and extrusion to obtain a heat-resistant flame-retardant microporous foamed polystyrene material finished product.
Compared with the prior art, the invention has the beneficial effects that:
The polystyrene material prepared by the invention takes polystyrene, functional auxiliary agent, synergistic auxiliary agent, composite foaming agent, lubricant, antioxidant and the like as raw materials, and is prepared by weighing the polystyrene, the functional auxiliary agent, the synergistic auxiliary agent, the composite foaming agent, the lubricant and the antioxidant, mixing the raw materials in mixing equipment, heating the raw materials in an extruder, and then obtaining a finished product of the heat-resistant flame-retardant microporous foaming polystyrene material through melting, mixing, foaming and extrusion; the polystyrene material prepared by the invention not only has excellent heat resistance, but also has excellent flame retardant property; and has high cell density, small cell size (diameter) and good foaming effect.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a statistical graph of initial decomposition temperatures according to the present invention;
FIG. 2 is a statistical graph of oxygen index according to the present invention.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides a heat-resistant flame-retardant microporous expanded polystyrene material, which is prepared from the following raw materials in parts by weight: 50 parts of polystyrene, 8 parts of functional auxiliary agents, 10 parts of synergistic auxiliary agents, 6 parts of composite foaming agents, 6 parts of lubricants and 3 parts of antioxidants.
In this example, polystyrene was purchased from Dongguan brocade group plasticizing Co., ltd (model B-MS).
Wherein, the preparation process of the functional auxiliary agent is as follows:
placing a proper amount of carbon nanospheres into a proper amount of hydrochloric acid with the mass concentration of 35% according to the solid-to-liquid ratio of 0.02g/mL, and treating for 240min at 60r/min and 60 ℃; cooling to room temperature, filtering, washing the obtained product with deionized water for 2 times, and treating the obtained washed product in an oven at 85 ℃ for 40min to obtain a first material;
placing a proper amount of modifier into a proper amount of deionized water according to a solid-to-liquid ratio of 0.018g/mL, mixing for 20min, and adding a proper amount of hydrochloric acid solution into the mixture to adjust the pH of the mixture to 6.2 to obtain a modified solution;
Ultrasonically dispersing a proper amount of silicon nitride in a proper amount of modified solution according to a solid-liquid ratio of 0.12g/mL, mixing for 20min, then treating for 120min at 40 ℃, carrying out suction filtration, and then treating for 100min in a drying oven at 65 ℃ to obtain a second material;
and (3) ultrasonically dispersing a proper amount of first material in a proper amount of deionized water according to a solid-liquid ratio of 0.24g/mL, mixing for 30min, adding a second material into the obtained first material solution, treating for 10min under the condition of 340r/min, treating for 300min under the condition of 100 ℃, filtering, washing for 3 times by using deionized water, and treating for 120min in an oven at 80 ℃ to obtain the functional auxiliary agent.
In this example, it is to be noted that the carbon nanospheres were purchased from north sco nanotechnology, inc. In su (model number BK 2019122701).
Further, 3-aminopropyl trimethoxy silane is selected as the modifier.
In addition, the addition amount of the second material was 2.5% of the mass of the first material solution.
Wherein, the preparation process of the synergistic auxiliary agent is as follows:
Placing a proper amount of melamine into a proper amount of glycol according to a solid-to-liquid ratio of 0.036g/mL, and mixing for 30min at 70 ℃ under the condition of 220r/min to obtain a first mixed solution;
placing a proper amount of beta- (N-phenylformamide) ethyl methyl aluminum phosphinate into a proper amount of first mixed solution according to a solid-to-liquid ratio of 0.012g/mL, and mixing for 10min at the temperature of 85 ℃ under the condition of 540r/min to obtain a second mixed solution;
Adding phosphoric acid into the obtained second mixed solution, mixing for 180min at 75 ℃ under 180r/min, cooling to room temperature after mixing, centrifuging for 4min at 8000r/min, washing the obtained centrifugal product with absolute ethyl alcohol for 2 times, and treating in an oven at 60 ℃ for 20h to obtain the synergistic auxiliary agent.
Further, the addition amount of phosphoric acid was 2.6% by mass of the second mixed solution.
Wherein the composite foaming agent consists of azodicarbonamide and stearate in the mass ratio of 0.3:1 are mixed and compounded.
Further, the stearate comprises zinc stearate, calcium stearate and barium stearate according to the mass ratio of 0.3:0.2:1 are mixed and compounded.
Wherein, the lubricant is polyethylene wax.
The antioxidant is selected from antioxidant 1010.
In addition, the embodiment also provides a preparation method of the heat-resistant flame-retardant microporous expanded polystyrene material, which comprises the following steps:
firstly, accurately weighing polystyrene, a functional auxiliary agent, a synergistic auxiliary agent, a composite foaming agent, a lubricant and an antioxidant respectively, and then placing the materials in mixing equipment to be mixed for 20 minutes at 170 ℃ to obtain a mixed material;
And step two, placing the obtained mixture into an extruder, heating to 200 ℃, and then carrying out melt mixing foaming and extrusion to obtain a heat-resistant flame-retardant microporous foamed polystyrene material finished product.
Example 2
The embodiment provides a heat-resistant flame-retardant microporous expanded polystyrene material, which is prepared from the following raw materials in parts by weight: 55 parts of polystyrene, 10 parts of functional auxiliary agents, 11 parts of synergistic auxiliary agents, 8 parts of composite foaming agents, 8 parts of lubricants and 4 parts of antioxidants.
In this example, polystyrene was purchased from Dongguan brocade group plasticizing Co., ltd (model B-MS).
Wherein, the preparation process of the functional auxiliary agent is as follows:
Placing a proper amount of carbon nanospheres into a proper amount of hydrochloric acid with the mass concentration of 35% according to the solid-to-liquid ratio of 0.03g/mL, and treating for 245min at the temperature of 62 ℃ at the speed of 65 r/min; after cooling to room temperature, carrying out suction filtration and washing the obtained product with deionized water for 4 times, and treating the obtained washed product in an oven at 90 ℃ for 45min to obtain a first material;
Placing a proper amount of modifier into a proper amount of deionized water according to a solid-to-liquid ratio of 0.02g/mL, mixing for 25min, and adding a proper amount of hydrochloric acid solution into the mixture to adjust the pH of the mixture to 6.3 to obtain a modified solution;
Ultrasonically dispersing a proper amount of silicon nitride in a proper amount of modified solution according to a solid-liquid ratio of 0.17g/mL, mixing for 25min, then treating for 130min at 41 ℃, and treating for 110min in an oven at 70 ℃ after suction filtration to obtain a second material;
And (3) ultrasonically dispersing a proper amount of first materials in a proper amount of deionized water according to a solid-liquid ratio of 0.26g/mL, mixing for 35min, adding a second material into the obtained first material solution, treating for 12min under the condition of 440r/min, treating for 310min under the condition of 105 ℃, filtering, washing for 4 times by using deionized water, and treating for 130min in an oven at 85 ℃ to obtain the functional auxiliary agent.
In this example, it is to be noted that the carbon nanospheres were purchased from north sco nanotechnology, inc. In su (model number BK 2019122701).
Further, the modifier is gamma-aminopropyl trimethoxy silane.
In addition, the addition amount of the second material was 3.5% of the mass of the first material solution.
Wherein, the preparation process of the synergistic auxiliary agent is as follows:
Placing a proper amount of melamine into a proper amount of glycol according to a solid-to-liquid ratio of 0.046g/mL, and mixing for 35min at 75 ℃ under the condition of 270r/min to obtain a first mixed solution;
Placing a proper amount of beta- (N-phenylformamide) ethyl methyl aluminum phosphinate into a proper amount of first mixed solution according to a solid-to-liquid ratio of 0.026g/mL, and mixing for 12min at 87 ℃ and 590r/min to obtain a second mixed solution;
Adding phosphoric acid into the obtained second mixed solution, mixing for 190min at 75 ℃ under 230r/min, cooling to room temperature after the mixing is finished, centrifuging for 5min under 10000r/min, washing the obtained centrifugal product with absolute ethyl alcohol for 4 times, and then treating in an oven at 62 ℃ for 23h to obtain the synergistic auxiliary agent.
Further, the addition amount of phosphoric acid was 3.2% of the mass of the second mixed solution.
Wherein the composite foaming agent consists of azodicarbonamide and stearate in the mass ratio of 0.4:1 are mixed and compounded.
Further, the stearate comprises zinc stearate, calcium stearate and barium stearate according to the mass ratio of 0.5:0.3:1 are mixed and compounded.
Wherein, the lubricant is polyethylene wax.
The antioxidant is antioxidant 168.
In addition, the embodiment also provides a preparation method of the heat-resistant flame-retardant microporous expanded polystyrene material, which comprises the following steps:
Firstly, accurately weighing polystyrene, a functional auxiliary agent, a synergistic auxiliary agent, a composite foaming agent, a lubricant and an antioxidant respectively, and then placing the materials in mixing equipment to be mixed for 25 minutes at 185 ℃ to obtain a mixed material;
and step two, placing the obtained mixture into an extruder, heating to 210 ℃, and then carrying out melt mixing foaming and extrusion to obtain a heat-resistant flame-retardant microporous foamed polystyrene material finished product.
Example 3
The embodiment provides a heat-resistant flame-retardant microporous expanded polystyrene material, which is prepared from the following raw materials in parts by weight: 60 parts of polystyrene, 12 parts of functional auxiliary agents, 12 parts of synergistic auxiliary agents, 10 parts of composite foaming agents, 10 parts of lubricants and 5 parts of antioxidants.
In this example, polystyrene was purchased from Dongguan brocade group plasticizing Co., ltd (model B-MS).
Wherein, the preparation process of the functional auxiliary agent is as follows:
Placing a proper amount of carbon nanospheres into a proper amount of hydrochloric acid with the mass concentration of 35% according to the solid-to-liquid ratio of 0.05g/mL, and treating for 250min at the temperature of 64 ℃ at the speed of 70 r/min; after cooling to room temperature, carrying out suction filtration and washing the obtained product with deionized water for 6 times, and treating the obtained washed product in an oven at 95 ℃ for 50min to obtain a first material;
placing a proper amount of modifier into a proper amount of deionized water according to a solid-to-liquid ratio of 0.024g/mL, mixing for 30min, and adding a proper amount of hydrochloric acid solution into the mixture to adjust the pH of the mixture to 6.5 to obtain a modified solution;
Ultrasonically dispersing a proper amount of silicon nitride in a proper amount of modified solution according to a solid-liquid ratio of 0.22g/mL, mixing for 30min, then treating for 140min at 42 ℃, carrying out suction filtration, and then treating for 120min in an oven at 75 ℃ to obtain a second material;
And (3) ultrasonically dispersing a proper amount of first materials in a proper amount of deionized water according to a solid-liquid ratio of 0.28g/mL, mixing for 40min, adding a second material into the obtained first material solution, treating for 15min under the condition of 540r/min, treating for 320min under the condition of 110 ℃, filtering, washing for 5 times by using deionized water, and treating for 140min in an oven at 90 ℃ to obtain the functional auxiliary agent.
In this example, it is to be noted that the carbon nanospheres were purchased from north sco nanotechnology, inc. In su (model number BK 2019122701).
Further, 3-glycidoxy propyl trimethoxy silane is selected as the modifier.
In addition, the addition amount of the second material was 4.5% of the mass of the first material solution.
Wherein, the preparation process of the synergistic auxiliary agent is as follows:
Placing a proper amount of melamine into a proper amount of glycol according to a solid-to-liquid ratio of 0.056g/mL, and mixing for 40min at 80 ℃ under the condition of 320r/min to obtain a first mixed solution;
Placing a proper amount of beta- (N-phenylformamide) ethyl methyl aluminum phosphinate into a proper amount of first mixed solution according to a solid-to-liquid ratio of 0.036g/mL, and mixing for 15min at 90 ℃ under the condition of 640r/min to obtain a second mixed solution;
Adding phosphoric acid into the obtained second mixed solution, mixing for 200min at 75 ℃ under the condition of 280r/min, cooling to room temperature after the mixing is finished, centrifuging for 6min under the condition of 12000r/min, washing the obtained centrifugal product with absolute ethyl alcohol for 8 times, and then treating in an oven at 65 ℃ for 26h to obtain the synergistic agent.
Further, the addition amount of phosphoric acid was 4.2% by mass of the second mixed solution.
Wherein the composite foaming agent consists of azodicarbonamide and stearate in the mass ratio of 0.6:1 are mixed and compounded.
Further, the stearate comprises zinc stearate, calcium stearate and barium stearate according to the mass ratio of 0.7:0.4:1 are mixed and compounded.
Wherein, the lubricant is oxidized polyethylene wax.
The antioxidant is antioxidant 168.
In addition, the embodiment also provides a preparation method of the heat-resistant flame-retardant microporous expanded polystyrene material, which comprises the following steps:
firstly, accurately weighing polystyrene, a functional auxiliary agent, a synergistic auxiliary agent, a composite foaming agent, a lubricant and an antioxidant respectively, and then placing the materials in mixing equipment to be mixed for 30min at 200 ℃ to obtain a mixed material;
And step two, placing the obtained mixture into an extruder, heating to 220 ℃, and then carrying out melt mixing foaming and extrusion to obtain a heat-resistant flame-retardant microporous foamed polystyrene material finished product.
Comparative example 1: the preparation method and the specific proportion of the raw materials of the polystyrene material provided by the embodiment are approximately the same as those of the embodiment 1, and the main differences are that: in this embodiment the functional auxiliary agent is replaced by a carbon nanosphere.
Comparative example 2: the preparation method and the specific proportion of the raw materials of the polystyrene material provided by the embodiment are approximately the same as those of the embodiment 1, and the main differences are that: in this example, no co-agent is contained.
Comparative example 3: the preparation method and the specific proportion of the raw materials of the polystyrene material provided by the embodiment are approximately the same as those of the embodiment 1, and the main differences are that: the complex blowing agent in this example is replaced by azodicarbonamide.
Effect testing
Polystyrene materials prepared by examples 1 to 3 in the present invention were respectively denoted as examples 1 to 3; the polystyrene materials prepared by comparative examples 1 to 3 were designated as comparative examples 1 to 3; the properties of the equivalent amount of each set of polystyrene material samples were then separately examined.
Test 1, heat resistance test and result analysis:
Measuring the heat resistance effect by adopting a thermogravimetric analyzer (TGA); the test conditions were as follows: taking 10mg of sample, heating up under nitrogen atmosphere, heating up to 30-750 ℃, heating up at a speed of 20 ℃/min, and recording a TGA curve. The relevant data are recorded in table 1.
As can be seen from table 1 and fig. 1, the polystyrene materials of examples 1 to 3 have excellent initial decomposition temperatures; at the same time, the differences between the example groups are not apparent. The above results indicate that the polystyrene materials of examples 1 to 3 have a remarkable high temperature resistant effect.
To verify the effect of the components of the present additive, tests of comparative examples 1 to 3 were set up.
The raw material ratios of the polystyrene materials of the comparative group 1 and the example 1 are mainly different in that the functional auxiliary agent is replaced by the carbon nanospheres. The initial decomposition temperature was found to be reduced by 50 ℃ in the comparative group 1 compared to the example 1 group. The result shows that the functional auxiliary agent plays an important role in improving the high temperature resistance of the polystyrene material.
The main difference between the raw material ratios of the polystyrene materials of the comparative group 2 and the polystyrene materials of the example 1 is that the polystyrene materials do not contain synergistic auxiliary agents. The initial decomposition temperature was found to be reduced by 15 ℃ for the comparative group 2 compared to the example 1 group. The result shows that the synergistic auxiliary agent has an effect on improving the high temperature resistance of the polystyrene material.
The main difference between the raw material ratios of the polystyrene materials of the comparative group 3 and the polystyrene materials of the example 1 is that the composite foaming agent is replaced by azodicarbonamide. The initial decomposition temperature was found to be reduced by 2 ℃ for the comparative group 3 compared to the example 1 group. The result shows that the composite foaming agent has little influence on improving the high temperature resistance of the polystyrene material.
Test 2, flame retardant test and result analysis:
the flame retardant performance of each set of polystyrene material samples was tested according to the detection standard of GB/T2406.2-2009, and the relevant data are recorded in Table 2.
As can be seen from table 2 and fig. 2, the polystyrene materials of examples 1 to 3 have excellent oxygen indexes; at the same time, the differences between the example groups are not apparent. The above results indicate that the polystyrene materials of examples 1 to 3 have a remarkable flame retardant effect.
To verify the effect of the components of the present additive, tests of comparative examples 1 to 3 were set up.
The raw material ratios of the polystyrene materials of the comparative group 1 and the example 1 are mainly different in that the functional auxiliary agent is replaced by the carbon nanospheres. The oxygen index was found to be reduced by 5% in the comparative group 1 compared to the example 1 group. The result shows that the functional auxiliary agent plays a role in improving the flame retardant property of the polystyrene material.
The main difference between the raw material ratios of the polystyrene materials of the comparative group 2 and the polystyrene materials of the example 1 is that the polystyrene materials do not contain synergistic auxiliary agents. The oxygen index was found to be reduced by 10% in the comparative group 2 compared to the example 1 group. The result shows that the synergistic auxiliary agent plays an important role in improving the flame retardant property of the polystyrene material.
The main difference between the raw material ratios of the polystyrene materials of the comparative group 3 and the polystyrene materials of the example 1 is that the composite foaming agent is replaced by azodicarbonamide. The oxygen index was found to be reduced by 0% in the comparative group 3 compared to the example 1 group. The result shows that the composite foaming agent has little influence on improving the flame retardant property of the polystyrene material.
Test 3, cell test and result analysis:
the cell morphology inside each group of styrene materials was analyzed by scanning electron microscopy, the average cell diameter was measured by Image-pro-plus Image analysis, and the relevant data was recorded in table 3.
As can be seen from Table 3, the polystyrene materials of examples 1 to 3 have smaller cell average diameters and higher cell densities; at the same time, the differences between the example groups are not apparent. The above results indicate that the polystyrene materials of examples 1 to 3 have the effects of high cell density, small cell size (diameter) and good foaming effect.
To verify the effect of the components of the present additive, tests of comparative examples 1 to 3 were set up.
The raw material ratios of the polystyrene materials of the comparative group 1 and the example 1 are mainly different in that the functional auxiliary agent is replaced by the carbon nanospheres. It was found that the average cell diameter of the comparative group 1 was increased by 1.7um and the cell density was reduced by 0.5X10 8Cells/cm3 as compared to the example 1 group. The results show that the functional auxiliary agent has an effect on the foaming performance of the polystyrene material.
The main difference between the raw material ratios of the polystyrene materials of the comparative group 2 and the polystyrene materials of the example 1 is that the polystyrene materials do not contain synergistic auxiliary agents. It was found that the average cell diameter of the comparative group 2 was increased by 0.2um and the cell density was decreased by 0.1X10 8Cells/cm3 as compared to the example 1 group. The result shows that the synergistic auxiliary agent has little influence on improving the foaming performance of the polystyrene material.
The main difference between the raw material ratios of the polystyrene materials of the comparative group 3 and the polystyrene materials of the example 1 is that the composite foaming agent is replaced by azodicarbonamide. It was found that the average cell diameter of the comparative group 3 was increased by 22um and the cell density was reduced by 1.84×10 8Cells/cm3 as compared to the group of example 1. The result shows that the composite foaming agent plays an important role in the foaming performance of the polystyrene material.
From the above, the polystyrene material prepared by the invention has excellent heat resistance and flame retardance; and has high cell density, small cell size (diameter) and good foaming effect. Therefore, the polystyrene material produced by the invention has wider market prospect and is more suitable for popularization.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (9)
1. A heat-resistant flame-retardant microporous expanded polystyrene material is characterized in that: the heat-resistant flame-retardant microporous expanded polystyrene material is prepared from the following raw materials in parts by weight: 50 to 60 parts of polystyrene, 8 to 12 parts of functional auxiliary agents, 10 to 12 parts of synergistic auxiliary agents, 6 to 10 parts of composite foaming agents, 6 to 10 parts of lubricants and 3 to 5 parts of antioxidants;
The preparation process of the functional auxiliary agent comprises the following steps:
Placing a proper amount of carbon nanospheres into a proper amount of hydrochloric acid with the mass concentration of 35% according to the solid-to-liquid ratio of 0.02-0.05 g/mL, and treating for 240-250 min under the conditions of 60-70 r/min and 60-64 ℃; cooling to room temperature, filtering, washing the obtained product with deionized water for 2-6 times, and treating the obtained washed product in an oven at 85-95 ℃ for 40-50 min to obtain a first material;
Placing a proper amount of modifier into a proper amount of deionized water according to a solid-to-liquid ratio of 0.018-0.024 g/mL, mixing for 20-30 min, adding a proper amount of hydrochloric acid solution into the mixture, and adjusting the pH of the mixture to 6.2-6.5 to obtain a modified solution;
dispersing a proper amount of silicon nitride in a proper amount of modified solution according to a solid-liquid ratio of 0.12-0.22 g/mL, mixing for 20-30 min, then treating for 120-140 min at 40-42 ℃, and treating for 100-120 min in an oven at 65-75 ℃ after suction filtration to obtain a second material;
Dispersing a proper amount of a first material in a proper amount of deionized water according to a solid-to-liquid ratio of 0.24-0.28 g/mL for mixing for 30-40 min, adding a second material into the obtained first material solution, treating for 10-15 min under the condition of 340-540 r/min, treating for 300-320 min under the condition of 100-110 ℃, filtering, washing for 3-5 times with deionized water, and treating for 120-140 min in an oven at 80-90 ℃ to obtain a functional auxiliary agent;
the preparation process of the synergistic auxiliary agent comprises the following steps:
placing a proper amount of melamine into a proper amount of glycol according to a solid-to-liquid ratio of 0.036-0.056 g/mL, and mixing for 30-40 min under the conditions of 70-80 ℃ and 220-320 r/min to obtain a first mixed solution;
placing a proper amount of beta- (N-phenylformamide) ethyl methyl aluminum phosphinate into a proper amount of first mixed solution according to a solid-to-liquid ratio of 0.012-0.036 g/mL, and mixing for 10-15 min at a temperature of 85-90 ℃ under a condition of 540-640 r/min to obtain a second mixed solution;
Adding phosphoric acid into the obtained second mixed solution, mixing for 180-200 min at the temperature of 75 ℃ under the condition of 180-280 r/min, cooling to room temperature after mixing, centrifuging for 4-6 min under the condition of 8000-12000 r/min, washing the obtained centrifugal product with absolute ethyl alcohol for 2-8 times, and then treating in an oven at the temperature of 60-65 ℃ for 20-26 h to obtain the synergistic auxiliary agent.
2. The heat-resistant flame-retardant microporous expanded polystyrene material according to claim 1, wherein: the modifier is any one of 3-aminopropyl trimethoxy silane, gamma-aminopropyl trimethoxy silane and 3-glycidol ether oxygen propyl trimethoxy silane.
3. The heat-resistant flame-retardant microporous expanded polystyrene material according to claim 1, wherein: the addition amount of the second material is 2.5-4.5% of the mass of the first material solution.
4. The heat-resistant flame-retardant microporous expanded polystyrene material according to claim 1, wherein: the adding amount of the phosphoric acid is 2.6-4.2% of the mass of the second mixed solution.
5. The heat-resistant flame-retardant microporous expanded polystyrene material according to claim 1, wherein: the composite foaming agent is prepared from azodicarbonamide and stearate in a mass ratio of 0.3-0.6: 1 are mixed and compounded.
6. The heat-resistant flame-retardant microporous expanded polystyrene material according to claim 5, wherein: the stearate is prepared from zinc stearate, calcium stearate and barium stearate according to the mass ratio of 0.3-0.7: 0.2 to 0.4:1 are mixed and compounded.
7. The heat-resistant flame-retardant microporous expanded polystyrene material according to claim 1, wherein: the lubricant is selected from any one of polyethylene wax and oxidized polyethylene wax.
8. The heat-resistant flame-retardant microporous expanded polystyrene material according to claim 1, wherein: the antioxidant is selected from any one of antioxidant 1010 and antioxidant 168.
9. The method for preparing a heat-resistant flame-retardant microporous expanded polystyrene material according to any one of claims 1 to 8, characterized by comprising the steps of:
Firstly, accurately weighing polystyrene, functional auxiliary agent, synergistic auxiliary agent, composite foaming agent, lubricant and antioxidant respectively, and then placing the materials in mixing equipment to mix for 20-30 min at 170-200 ℃ to obtain a mixed material;
and step two, placing the obtained mixture into an extruder, heating to 200-220 ℃, and then performing melt mixing foaming and extrusion to obtain a heat-resistant flame-retardant microporous foamed polystyrene material finished product.
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