CN105778264B - Preparation method of halogen-free flame-retardant POE material - Google Patents
Preparation method of halogen-free flame-retardant POE material Download PDFInfo
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- CN105778264B CN105778264B CN201610262417.4A CN201610262417A CN105778264B CN 105778264 B CN105778264 B CN 105778264B CN 201610262417 A CN201610262417 A CN 201610262417A CN 105778264 B CN105778264 B CN 105778264B
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 48
- 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 46
- 239000000463 material Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000004114 Ammonium polyphosphate Substances 0.000 claims abstract description 23
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims abstract description 23
- 229920001276 ammonium polyphosphate Polymers 0.000 claims abstract description 23
- 239000002131 composite material Substances 0.000 claims abstract description 22
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 17
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 17
- ZQKXQUJXLSSJCH-UHFFFAOYSA-N melamine cyanurate Chemical compound NC1=NC(N)=NC(N)=N1.O=C1NC(=O)NC(=O)N1 ZQKXQUJXLSSJCH-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229920005989 resin Polymers 0.000 claims abstract description 12
- 239000011347 resin Substances 0.000 claims abstract description 12
- BPXVHIRIPLPOPT-UHFFFAOYSA-N 1,3,5-tris(2-hydroxyethyl)-1,3,5-triazinane-2,4,6-trione Chemical compound OCCN1C(=O)N(CCO)C(=O)N(CCO)C1=O BPXVHIRIPLPOPT-UHFFFAOYSA-N 0.000 claims abstract description 9
- 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 abstract description 9
- 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 abstract description 8
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 2
- 238000001125 extrusion Methods 0.000 claims description 2
- 238000005469 granulation Methods 0.000 claims description 2
- 230000003179 granulation Effects 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 claims description 2
- 150000003863 ammonium salts Chemical class 0.000 claims 1
- 230000032683 aging Effects 0.000 abstract description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 4
- 238000002485 combustion reaction Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- 239000001301 oxygen Substances 0.000 abstract description 4
- 229920006124 polyolefin elastomer Polymers 0.000 description 39
- 230000000052 comparative effect Effects 0.000 description 16
- 238000012360 testing method Methods 0.000 description 6
- 239000003607 modifier Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 239000003094 microcapsule Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
-
- 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
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
- C08K5/134—Phenols containing ester groups
- C08K5/1345—Carboxylic esters of phenolcarboxylic acids
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3477—Six-membered rings
- C08K5/3492—Triazines
- C08K5/34924—Triazines containing cyanurate groups; Tautomers thereof
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
- C08K5/526—Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl compounds
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
-
- 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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
Abstract
The invention discloses a halogen-free flame-retardant POE material and a preparation method thereof, wherein the halogen-free flame-retardant POE material is prepared from the following components in parts by weight: 100 parts of POE resin, 25-60 parts of halogen-free composite flame retardant and 0.1-1.0 part of antioxidant. The halogen-free composite flame retardant consists of active ammonium polyphosphate (APP), Melamine Cyanuric Acid (MCA) and tris (2-hydroxyethyl) isocyanurate in a weight ratio of 100: 8-20. The antioxidant is a composite antioxidant which is composed of an antioxidant 1010 and an antioxidant 168 according to the weight ratio of 1: 1-1: 3. The halogen-free flame-retardant POE material has a good flame-retardant effect (the oxygen index is greater than 30, and the vertical combustion V-0 level), has high mechanical properties, particularly has a breaking elongation of more than 850%, and also has good heat aging resistance.
Description
The invention is a divisional application of an invention patent application with the application number of 201410391702.7 and the application date of 2014, 8 and 11, and the invention is named as a halogen-free flame-retardant POE material and a preparation method thereof.
Technical Field
The invention relates to a high polymer material and a preparation method thereof, and particularly relates to a halogen-free flame-retardant POE material and a preparation method thereof.
Background
The POE resin is a novel polyolefin elastomer polymerized by the Dow chemical company in America by taking metallocene as a catalyst, has the advantages of low price, easy molding and processing and the like compared with other polyolefin elastomers, and is widely applied to the fields of automobiles, electronic appliances, building sealing, sports equipment, toughening and modification of polymers and the like.
POE belongs to flammable materials, and with the increasing application of POE, flame retardant modification of POE is imperative.
Chinese patent document CN102585346A discloses a halogen-free flame-retardant POE composite material, which is prepared from POE resin, a halogen-free composite flame retardant, a modifier, a lubricating dispersant and an antioxidant, wherein the halogen-free composite flame retardant is composed of active magnesium hydroxide/active aluminum hydroxide, zinc borate and microcapsule red phosphorus, and the antioxidant is single antioxidant 1010. The halogen-free flame-retardant POE composite material has the following defects: (1) the flame retardant with the dosage higher than that of POE (polyolefin elastomer) is used for obtaining a better flame retardant effect, so that the mechanical property of the POE composite material is reduced, a modifier is needed for improving the mechanical property of the material, and meanwhile, the proportion of the POE composite material is increased, so that the production cost is further increased. (2) With the addition of modifiers, the elongation at break is still low (less than 650%), so that the use is somewhat limited. (3) The heat aging resistance is poor, the tensile strength change rate is more than 10 percent and the elongation at break change rate is more than 15 percent after aging for 168 hours at 80 ℃.
Disclosure of Invention
One of the purposes of the present invention is to solve the above problems and provide a halogen-free flame retardant POE material which has a good flame retardant effect, a low production cost, a good mechanical property, and no need of any modifier.
The invention also aims to provide a preparation method of the halogen-free flame-retardant POE material.
The technical scheme for realizing one purpose of the invention is as follows: a halogen-free flame-retardant POE material is prepared from the following components in parts by weight: 100 parts of POE resin, 25-60 parts of halogen-free composite flame retardant and 0.1-1.0 part of antioxidant; preferably 100 parts of POE resin, 35-40 parts of halogen-free composite flame retardant and 0.2-0.5 part of antioxidant.
The halogen-free composite flame retardant consists of active ammonium polyphosphate (APP), Melamine Cyanuric Acid (MCA) and tris (2-hydroxyethyl) isocyanurate in a weight ratio of 100: 8-20.
The active ammonium polyphosphate is obtained by modifying ammonium polyphosphate by using a silane coupling agent, wherein the weight ratio of the ammonium polyphosphate to the silane coupling agent is 100: 2-100: 4.
In order to improve the heat aging resistance of the halogen-free flame-retardant POE material, the antioxidant is preferably a composite antioxidant consisting of an antioxidant 1010 and an antioxidant 168 according to the weight ratio of 1: 1-1: 3.
the preparation method of the halogen-free flame-retardant POE material comprises the following steps of pouring POE resin, active ammonium polyphosphate, melamine cyanuric acid, tris (2-hydroxyethyl) isocyanurate and an antioxidant which are weighed according to a formula into a high-speed mixer to be mixed until the temperature of the material rises to 65-75 ℃ due to friction heat generated by mixing, discharging and cooling, ② feeding the cooled mixed material into a double-screw extruder to be melted and extruded, and cooling and drawing the extruded strips into a granulator to be granulated to obtain the halogen-free flame-retardant POE material.
the antioxidant in the step ① is a composite antioxidant which is composed of an antioxidant 1010 and an antioxidant 168 according to the weight ratio of 1: 1-1: 3.
the active ammonium polyphosphate is obtained by modifying ammonium polyphosphate by using a silane coupling agent, wherein the weight ratio of the ammonium polyphosphate to the silane coupling agent is 100: 2-100: 4.
in step ②, the temperature of each zone of the double-screw extruder is T1=80℃~85℃,T2=85℃~90℃,T3=90℃~100℃,T4=100~110℃,T5=110~120℃,T6=120~130℃,T7=130~140℃,T8=140~145℃,T9=130~140℃,TDie=135~140℃。
The invention has the following positive effects: (1) the halogen-free flame-retardant POE material disclosed by the invention adopts a halogen-free composite flame-retardant system consisting of active ammonium polyphosphate, melamine cyanuric acid and tris (2-hydroxyethyl) isocyanurate, and the halogen-free composite flame-retardant system can obtain a better flame-retardant effect (the oxygen index is greater than 30 and the vertical combustion V-0 level) only by using a small amount, so that the production cost is reduced, and in addition, the material still has higher mechanical properties without a modifier, especially the elongation at break can reach more than 850%, so that the halogen-free composite flame-retardant POE material has wider application. (2) The halogen-free flame-retardant POE material adopts the hindered phenol antioxidant 1010 and the phosphite antioxidant 168 to form the composite antioxidant, so that the heat aging resistance of the material can be greatly improved, the material is aged for 168 hours at the temperature of 80 ℃, and the change rate of the tensile strength and the elongation at break is less than 5 percent.
Detailed Description
(example 1)
The halogen-free flame-retardant POE material of the embodiment is prepared from the following components in parts by weight:
100kg of POE resin, 28kg of active ammonium polyphosphate, 4kg of melamine cyanurate, 4kg of tris (2-hydroxyethyl) isocyanurate, 0.1kg of antioxidant 1010 and 0.3kg of antioxidant 168.
The preparation method of the halogen-free flame-retardant POE material comprises the following steps:
firstly, 200kg of ammonium polyphosphate and 5kg of silane coupling agent with the trade name of KH-560 produced by Nanjing Aucheng chemical Limited company are poured into a high-speed mixer with the rotating speed of 900 revolutions per minute to be mixed for 6min, the friction heat generated by mixing at the moment enables the temperature of the materials to rise to 85 ℃, and the materials are discharged and cooled to obtain the active ammonium polyphosphate.
28kg of the active ammonium polyphosphate prepared above, 100kg of POE resin, 4kg of melamine cyanurate, 4kg of tris (2-hydroxyethyl) isocyanurate, 0.1kg of antioxidant 1010 and 0.3kg of antioxidant 168 are poured into a high-speed mixer at the rotating speed of 900 revolutions per minute to be mixed until the temperature of the materials is raised to 70 ℃ by the friction heat generated by mixing (at the moment, the flame retardant and the antioxidant are both adhered to the surface of the POE particles), and the mixture is discharged and cooled to room temperature (15-25 ℃).
②, feeding the cooled mixed material into a double-screw extruder for melt extrusion, and cooling the extruded strip material by a water tank, drawing the cooled strip material into a granulator for granulation to obtain the halogen-free flame-retardant POE material.
The temperature of each zone of the double-screw extruder is as follows: t is1=80℃~85℃,T2=85℃~90℃,T3=90℃~100℃,T4=100~110℃,T5=110~120℃,T6=120~130℃,T7=130~140℃,T8=140~145℃,T9=130~140℃,TDie=135~140℃。
(examples 2 to 6)
The preparation method of each example is the same as that of example 1, except for the weight ratio of each component, which is shown in Table 1.
TABLE 1
Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | |
POE resin | 100kg | 100kg | 100kg | 100kg | 100kg | 100kg |
Active ammonium polyphosphate | 28kg | 30kg | 32kg | 30kg | 28kg | 28kg |
Melamine cyanuric acid | 4kg | 3kg | 4kg | 5kg | 4kg | 4kg |
Tris (2-hydroxyethyl) isocyanurate | 4kg | 4kg | 4kg | 5kg | 4kg | 4kg |
Antioxidant 1010 | 0.1kg | 0.1kg | 0.2kg | 0.1kg | 0.2kg | - |
Antioxidant 168 | 0.3kg | 0.2kg | 0.3kg | 0.2kg | - | 0.2kg |
(application example)
The halogen-free flame-retardant POE materials prepared in the embodiments 1 to 6 are added into a double-roller open mill to plasticate a pulling-on piece, the pulling-on piece is tabletted and formed on a tablet press, a standard sample is prepared by adopting a plastic standard sample preparation machine, the mechanical property and the flame retardant property of the standard sample and the mechanical property after aging at 80 ℃ for 168 hours are tested according to the national standard, and the test results are shown in Table 2.
TABLE 2
Testing performance | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 |
Tensile strength/MPa | 12.6 | 13.0 | 13.2 | 12.8 | 12.1 | 12.2 |
Elongation at break/% | 907 | 870 | 868 | 884 | 850 | 845 |
Oxygen index/% | 31 | 33 | 34 | 36 | 31 | 31 |
Vertical combustion | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 |
Tensile strength/MPa (after aging) | 12.8 | 13.1 | 13.4 | 12.5 | 11.1 | 11.2 |
Elongation at break/% (after aging) | 875 | 856 | 845 | 872 | 761 | 765 |
(comparative examples 1 to 5)
The preparation method of each proportion is the same as that of the example 1, except that the weight ratio of the halogen-free composite flame retardant is shown in the table 3.
TABLE 3
Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | |
POE resin | 100kg | 100kg | 100kg | 100kg | 100kg |
Active ammonium polyphosphate | 14kg | 56kg | 28kg | 28kg | 28kg |
Melamine cyanuric acid | 2kg | 8kg | 4kg | - | - |
Tris (2-hydroxyethyl) isocyanurate | 2kg | 8kg | - | 4kg | - |
Antioxidant 1010 | 0.1kg | 0.1kg | 0.1kg | 0.1kg | 0.1kg |
Antioxidant 168 | 0.1kg | 0.1kg | 0.1kg | 0.1kg | 0.1kg |
Comparative example 6
The comparative example is the halogen-free flame-retardant POE composite material prepared in example 1 of Chinese patent document CN 102585346A.
(comparative application example)
And adding the halogen-free flame-retardant POE materials prepared in the comparative examples 1 to 6 into a double-roller open mill to plasticate a pulling-on piece, tabletting and forming on a tablet press, preparing a standard sample by using a plastic standard sample preparation machine, testing the mechanical property and the flame retardant property of the standard sample according to the national standard, and testing the mechanical property after aging at 80 ℃ for 168 hours, wherein the test results are shown in Table 4.
TABLE 4
Testing performance | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 |
Tensile strength/MPa | 13.6 | 10.1 | 12.1 | 12.2 | 12.2 | 12.6 |
Elongation at break/% | 930 | 730 | 832 | 830 | 810 | 650 |
Oxygen index/% | 28 | 36 | 30 | 30 | 29 | 31.5 |
Vertical combustion | V-2 | V-0 | V-1 | V-1 | V-1 | V-0 |
Tensile strength/MPa (after aging) | 13.1 | 10.4 | 11.7 | 12.5 | 11.8 | 11.1 |
Elongation at break/% (after aging) | 902 | 705 | 801 | 801 | 794 | 540 |
Claims (1)
1. A preparation method of a halogen-free flame-retardant POE material is characterized by comprising the following steps:
the halogen-free flame retardant POE material is prepared from the following components, by weight, 100 parts of POE resin, 35-40 parts of a halogen-free composite flame retardant and 0.2-0.5 part of an antioxidant, wherein the halogen-free composite flame retardant is prepared from active ammonium polyphosphate, melamine cyanuric acid and tris (2-hydroxyethyl) isocyanurate in a weight ratio of 100: 8-20, the antioxidant is prepared from antioxidant 1010 and antioxidant 168 in a weight ratio of 1: 1-1: 3, the active ammonium polyphosphate is prepared from silane coupling agent modified ammonium polyphosphate, and the weight ratio of the ammonium polyphosphate to the silane coupling agent is 100: 2-100: 4;
pouring the POE resin, the active ammonium polyphosphate, the melamine cyanuric acid, the tris (2-hydroxyethyl) isocyanurate and the antioxidant which are weighed according to the formula into a high-speed mixer for mixing until the friction heat generated by mixing raises the temperature of the materials to 65-75 ℃, discharging and cooling;
and secondly, feeding the cooled mixed material into a double-screw extruder for melt extrusion, cooling the extruded strip material by a water tank, and drawing the cooled strip material into a granulator for granulation to obtain the halogen-free flame-retardant POE material.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CN201610262417.4A CN105778264B (en) | 2014-08-11 | 2014-08-11 | Preparation method of halogen-free flame-retardant POE material |
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Application Number | Priority Date | Filing Date | Title |
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CN201610262417.4A CN105778264B (en) | 2014-08-11 | 2014-08-11 | Preparation method of halogen-free flame-retardant POE material |
CN201410391702.7A CN104140586B (en) | 2014-08-11 | 2014-08-11 | Halogen-free flameproof POE material and preparation method thereof |
Related Parent Applications (1)
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CN201410391702.7A Division CN104140586B (en) | 2014-08-11 | 2014-08-11 | Halogen-free flameproof POE material and preparation method thereof |
Publications (2)
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CN105778264A CN105778264A (en) | 2016-07-20 |
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CN101550249A (en) * | 2008-04-02 | 2009-10-07 | 上海化工研究院 | Halogen-free expandable fire retardant fiber glass reinforced polypropylene material and preparation method thereof |
CN102585346A (en) * | 2012-02-29 | 2012-07-18 | 江苏技术师范学院 | Halogen-free flame-retardant POE (Polyolefin Elastomer) compound material and preparation method thereof |
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CN1556136A (en) * | 2003-12-30 | 2004-12-22 | 上海化工研究院 | Halogen less expansion type polyolefine incombustible agent and its preparation method |
CN101550249A (en) * | 2008-04-02 | 2009-10-07 | 上海化工研究院 | Halogen-free expandable fire retardant fiber glass reinforced polypropylene material and preparation method thereof |
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Effective date of registration: 20201127 Address after: No.12 Yuanda Road, Guanlin Town, Yixing City, Wuxi City, Jiangsu Province Patentee after: Wuxi Linfeng cable new material Co., Ltd Address before: 213001 Changzhou Province in the Clock Tower District, Jiangsu, Wu Road, No. 1801 Patentee before: JIANGSU University OF TECHNOLOGY |