CN111621094A - Halogen-free synergistic flame-retardant modified EP-TPV material and preparation method thereof - Google Patents
Halogen-free synergistic flame-retardant modified EP-TPV material and preparation method thereof Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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Abstract
The invention provides a halogen-free synergistic flame-retardant modified EP-TPV material and a preparation method thereof. According to the invention, after the EP-TPV composite material and the halogen-free synergistic flame-retardant master batch formula thereof are optimized, the EP-TPV composite material with high flame-retardant efficiency is prepared in a reaction extrusion mode, the rigidity of the system is slightly improved on the premise of obviously improving the flame-retardant performance of the composite material, and the elastomer performance of the raw material can be maintained to a greater extent. The method is simple, easy to implement, low in cost and good in using effect.
Description
Technical Field
The invention relates to the technical field of ethylene propylene diene monomer/polypropylene (EPDM/PP) thermoplastic elastomers, in particular to a halogen-free synergistic flame-retardant composite material and a preparation method thereof.
Background
The EPDM/PP thermoplastic elastomer (hereinafter referred to as EP-TPV) has excellent mechanical property, weather resistance, insulativity, good processability and recyclability, is one of the thermoplastic elastomers with the largest dosage at present, has wide application prospect, but has extremely poor flame retardant property, and is greatly limited to the application in the field with higher flame retardant requirement. At present, certain results are obtained in the flame retardant research of EP-TPV, but some problems also exist: for example, the traditional inorganic flame retardant particles are modified, and the addition amount is large, so that the mechanical property of EP-TPV is greatly influenced; IFR particles prepared in a compound mode are easy to agglomerate into large particles, and the problem of system mechanical property deterioration also exists; the traditional halogen flame-retardant system has a relatively excellent flame-retardant effect, but has the problems of environmental protection and the like.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide a halogen-free synergistic flame-retardant EP-TPV modification method. The halogen-free synergistic flame-retardant EP-TPV material can keep the original mechanical properties to a higher degree on the basis of obviously improving the flame-retardant property of the material. The invention also aims to provide a convenient and efficient halogen-free flame-retardant EP-TPV modification method, which has the advantages of simple process, convenient operation and control, stable quality, high production efficiency and low production cost and can be used for large-scale industrial production.
The purpose of the invention is realized by the following technical scheme: a halogen-free synergistic flame-retardant modified EP-TPV material comprises the following raw materials in parts by weight:
26.4-28.8 parts of Ethylene Propylene Diene Monomer (EPDM)
39.6-43.2 Parts of Polypropylene (PP)
Pentaerythritol (PER) 12.68 parts
12.32 portions of Melamine Phosphate (MP)
3-9 parts of Zinc Borate (ZB)
And other processing aids including naphthenic oils and DCP crosslinkers
The invention firstly prepares EP-T by the conventional dynamic vulcanization modeA PV matrix material. Then passing through PER (C) with constant proportion5H12O4) And MP (C)3H9N6PO4) The halogen-free synergistic flame retardant EP-TPV is prepared by taking ZB as a synergistic flame retardant, performing melt blending on the ZB and a PP matrix in a reaction extrusion mode to prepare a flame retardant master batch, and finally performing melt blending on the matrix and the flame retardant master batch in an extrusion mode to prepare the halogen-free synergistic flame retardant EP-TPV.
The flame retardant property of EP-TPV can be obviously improved through the action of the halogen-free flame retardant master batch extruded by reaction and the ZB synergist: the UL-94 vertical burning grade is improved from no grade to V0 grade, the limiting oxygen index is improved from 18.5 to 30.1, and the initial thermal degradation temperature is increased from 273.0oC is maximally lifted to 417.5oC。
The halogen-free synergistic flame-retardant EP-TPV material can improve the rigidity of a system on the basis of obviously improving the flame-retardant property of the material, and can keep the mechanical property of the material to a greater extent: the tensile strength is reduced from 20.5MPa to 16.4MPa at most; the bending strength is improved from 8.5MPa to 26.7MPa at most; the elongation at break dropped from 550% to an average of 347%. The rigidity of the system is improved, the material can still keep the characteristics of the TPV elastomer, and the material has good processability and excellent comprehensive performance.
Preferably, the EPDM ethylene content is 60-70%, the mooney viscosity is 70;
preferably, the PP has a density of 0.9kg/m3Melt index of 2.9-3.5g/10min, Vicat softening point of 153oC；
Preferably, the PER is a standard pure product with a relative molar mass of 136 and a boiling point of 357.85oC。
Preferably, the MP contains more than or equal to 12 percent of phosphorus, more than or equal to 36 percent of nitrogen and 1.8 to 1.9g/cm of density3。
Preferably, the ZB is a pure standard substance with a relative molar mass of 125 and a melting point of 980oC, the particle size is 1-2 μm.
The temperature can be regulated and controlled by the MP and the PER with the parameters to generate the following reactions in the extrusion process:
the melamine salt of pentaerythritol phosphate containing (P = O) -O-C structure is generated, and has higher flame retardant efficiency compared with a MP and PER blended flame retardant formula. ZB, acting simultaneously in synergy, as an inorganic particle, degradable into stable boron oxide (B) during heating2O3) And can be attached to the surface of polymer to form a covering layer to limit the generation and oxidation reaction of combustible gas. On the other hand, the introduction of the synergist can also reduce the addition amount of an original intumescent flame retardant system in the composite material, and the flame retardant property of the composite material can be remarkably improved and higher mechanical property can be kept under the synergistic effects.
A preparation method of a halogen-free synergistic flame-retardant modified EP-TPV material comprises the following steps:
(1) the EPDM was placed at 70oC, drying in a constant-temperature drying oven for 8 hours, and then filling oil (naphthenic oil with 30 percent of rubber content) for 24 hours at room temperature; PP was also placed at 70oC, drying in a constant-temperature drying box for 8 hours;
(2) 26.4 to 28.8 portions of EPDM, 14.6 to 18.2 portions of PP and DCP crosslinking agent with the rubber content of 1.2 weight percent are put into a double-screw extruder for extrusion processing to prepare the EP-TPV matrix, the rotating speed of a main machine screw is 250r/min, the processing temperature is 185-oC；
(3) Placing MP, PER, ZB and PP at 70oC, drying in a constant-temperature drying box for 8 hours; then, 12.68 parts of PER, 12.32 parts of MP, 3-9 parts of ZB and 25 parts of PP are mixed evenly and then are extruded to prepare the flame-retardant master batch by reaction, and the processing temperature is controlled to 260-oC, the rotating speed of the screw is 200 r/min;
(4) uniformly mixing the synergistic flame-retardant master batch in the step (3) and the EP-TPV substrate in the step (2), extruding and granulating by a double-screw extruder, and finally controlling the rubber-plastic ratio in the composite material to be 40/60 (containing 26.4-28.8 parts of EPDM and 39.6-43.2 parts of PP), the content of the reactive flame retardant to be 25 percent and the content of the synergistic agent to be 3-9 percent; the rotation speed of the screw of the host machine is 250r/min, and the processing temperature is 185-oC, after shearing and mixing of an extruder, melting and compounding materials, finally extruding, cooling and granulating to obtain the productAnd (5) preparing the product.
The preparation method has simple process, the reaction extrusion process only needs to adjust the extrusion temperature, the operation and the control are convenient, the quantity is stable, the production efficiency is high, the production cost is low, and the large-scale industrial production can be realized.
The invention has the beneficial effects that: the halogen-free flame-retardant system after the MP/PER reaction extrusion in the invention is reacted with the inorganic particle ZB of the synergist, so that the flame-retardant property of EP-TPV is obviously improved, the rigidity of the composite material is improved, and the mechanical property and the property of the elastomer of the composite material can be maintained to a greater extent.
Detailed Description
The present invention is further illustrated below by way of examples to facilitate understanding by those skilled in the art, and the present invention is not limited to the examples mentioned in the embodiments.
Examples 1
The preparation method of the halogen-free synergistic flame-retardant EP-TPV composite material comprises the following raw materials in parts by weight:
ethylene Propylene Diene Monomer (EPDM) 28.8 parts
43.2 Parts of Polypropylene (PP)
Pentaerythritol (PER) 12.68 parts
12.32 portions of Melamine Phosphate (MP)
3 portions of Zinc Borate (ZB)
And other processing aids including naphthenic oils and DCP crosslinkers
The EPDM has an ethylene content of 60-70% and a Mooney viscosity of 70;
the PP density is 0.9kg/m3Melt index of 2.9-3.5g/10min, Vicat softening point of 153oC；
The PER is standard pure substance with the relative molar mass of 136 and the boiling point of 357.85oC。
The MP contains phosphorus more than or equal to 12 percent, nitrogen more than or equal to 36 percent and density of 1.8-1.9g/cm3。
The ZB is a standard pure substance, the relative molar mass is 125, and the melting point is 980oC。
A preparation method of a halogen-free synergistic flame-retardant modified EP-TPV material comprises the following steps:
(1) the EPDM was placed at 70oC, drying in a constant-temperature drying oven for 8 hours, and then filling oil (naphthenic oil with 30 percent of rubber content) for 24 hours at room temperature; PP was also placed at 70oC, drying in a constant-temperature drying box for 8 hours;
(2) 28.8 parts of EPDM, 18.2 parts of PP and DCP crosslinking agent with the rubber content of 1.2wt% are placed in a double-screw extruder for extrusion processing to prepare the EP-TPV matrix, the rotating speed of a main machine screw is 250r/min, and the processing temperature is 185-200-oC；
(3) Placing MP, PER, ZB and PP at 70oC, drying in a constant-temperature drying box for 8 hours; placing MP, PER, ZB and PP at 70oC, drying in a constant-temperature drying box for 8 hours; then uniformly mixing PER12.68 parts, MP12.32 parts, ZB3 parts and PP25 parts, performing reaction extrusion to prepare the flame-retardant master batch, and controlling the processing temperature to 260-oC, the rotating speed of the screw is 200 r/min;
(4) uniformly mixing the EP-TPV matrix in the step (2) and the synergistic flame-retardant master batch in the step (3) according to the formula ratio, extruding and granulating the mixture by a double-screw extruder to prepare halogen-free synergistic flame-retardant EP-TPV granules, wherein the rotating speed of a main machine screw is 250r/min, and the processing temperature is 185-oC。
EXAMPLES example 2
The preparation method of the halogen-free synergistic flame-retardant EP-TPV composite material comprises the following raw materials in parts by weight:
ethylene Propylene Diene Monomer (EPDM) 26.4 parts
39.6 Portions of Polypropylene (PP)
Pentaerythritol (PER) 12.68 parts
12.32 portions of Melamine Phosphate (MP)
4.5 parts of Zinc Borate (ZB)
The material selection type is the same as that of the example (1);
a preparation method of a halogen-free synergistic flame-retardant modified EP-TPV material comprises the following steps:
(1) the EPDM was placed at 70oC, drying in a constant-temperature drying oven for 8 hours, and then filling oil (naphthenic oil with 30 percent of rubber content) for 24 hours at room temperature; PP was also placed at 70oC, drying in a constant-temperature drying box for 8 hours;
(2) get28.2 parts of EPDM, 17.3 parts of PP and a DCP crosslinking agent with the rubber content of 1.2wt% are placed in a double-screw extruder for extrusion processing to prepare the EP-TPV matrix, the rotating speed of a main machine screw is 250r/min, and the processing temperature is 185-oC；
(3) Placing MP, PER, ZB and PP at 70oC, drying in a constant-temperature drying box for 8 hours; placing MP, PER, ZB and PP at 70oC, drying in a constant-temperature drying box for 8 hours; then, 12.68 parts of PER, 12.32 parts of MP, 4.5 parts of ZB and 25 parts of PP are mixed uniformly and then are reacted and extruded to prepare the flame-retardant master batch, and the processing temperature is controlled to 260-oC, the rotating speed of the screw is 200 r/min;
(4) uniformly mixing the EP-TPV matrix in the step (2) and the synergistic flame-retardant master batch in the step (3) according to the formula ratio, extruding and granulating the mixture by a double-screw extruder to prepare halogen-free synergistic flame-retardant EP-TPV granules, wherein the rotating speed of a main machine screw is 250r/min, and the processing temperature is 185-oC。
EXAMPLE 3
The preparation method of the halogen-free synergistic flame-retardant EP-TPV composite material comprises the following raw materials in parts by weight:
ethylene Propylene Diene Monomer (EPDM) 27.6 parts
41.4 Parts of Polypropylene (PP)
Pentaerythritol (PER) 12.68 parts
12.32 portions of Melamine Phosphate (MP)
6 portions of Zinc Borate (ZB)
The material selection category is as in example (1);
a preparation method of a halogen-free synergistic flame-retardant modified EP-TPV material comprises the following steps:
(1) the EPDM was placed at 70oC, drying in a constant-temperature drying oven for 8 hours, and then filling oil (naphthenic oil with 30 percent of rubber content) for 24 hours at room temperature; PP was also placed at 70oC, drying in a constant-temperature drying box for 8 hours;
(2) placing 27.6 parts of EPDM, 16.4 parts of PP and a DCP crosslinking agent with the rubber content of 1.2wt% in a double-screw extruder for extrusion processing to prepare the EP-TPV matrix, wherein the rotating speed of a main machine screw is 250r/min, and the processing temperature is 185-200-oC；
(3) Placing MP, PER, ZB and PP inAt 70oC, drying in a constant-temperature drying box for 8 hours; placing MP, PER, ZB and PP at 70oC, drying in a constant-temperature drying box for 8 hours; then uniformly mixing PER12.68 parts, MP12.32 parts, ZB6 parts and PP25 parts, performing reaction extrusion to prepare the flame-retardant master batch, and controlling the processing temperature to 260-oC, the rotating speed of the screw is 200 r/min;
(4) uniformly mixing the EP-TPV matrix in the step (2) and the synergistic flame-retardant master batch in the step (3) according to the formula ratio, extruding and granulating the mixture by a double-screw extruder to prepare halogen-free synergistic flame-retardant EP-TPV granules, wherein the rotating speed of a main machine screw is 250r/min, and the processing temperature is 185-oC。
EXAMPLE 4
The preparation method of the halogen-free synergistic flame-retardant EP-TPV composite material comprises the following raw materials in parts by weight:
ethylene Propylene Diene Monomer (EPDM) 26.4 parts
39.6 Portions of Polypropylene (PP)
Pentaerythritol (PER) 12.68 parts
12.32 portions of Melamine Phosphate (MP)
7.5 parts of Zinc Borate (ZB)
The material selection type is the same as that of the example (1);
a preparation method of a halogen-free synergistic flame-retardant modified EP-TPV material comprises the following steps:
(1) the EPDM was placed at 70oC, drying in a constant-temperature drying oven for 8 hours, and then filling oil (naphthenic oil with 30 percent of rubber content) for 24 hours at room temperature; PP was also placed at 70oC, drying in a constant-temperature drying box for 8 hours;
(2) placing 27 parts of EPDM, 15.5 parts of PP and a DCP crosslinking agent with the rubber content of 1.2wt% in a double-screw extruder for extrusion processing to prepare the EP-TPV matrix, wherein the rotating speed of a main machine screw is 250r/min, and the processing temperature is 185-oC；
(3) Placing MP, PER, ZB and PP at 70oC, drying in a constant-temperature drying box for 8 hours; placing MP, PER, ZB and PP at 70oC, drying in a constant-temperature drying box for 8 hours; then, 12.68 parts of PER, 12.32 parts of MP, 7.5 parts of ZB and 25 parts of PP are mixed uniformly and then are reacted and extruded to prepare the flame-retardant master batch, and the processing temperature is controlled to 260-oC, the rotating speed of the screw is 200 r/min;
(4) uniformly mixing the EP-TPV matrix in the step (2) and the synergistic flame-retardant master batch in the step (3) according to the formula ratio, extruding and granulating the mixture by a double-screw extruder to prepare halogen-free synergistic flame-retardant EP-TPV granules, wherein the rotating speed of a main machine screw is 250r/min, and the processing temperature is 185-oC。
EXAMPLE 5
The preparation method of the halogen-free synergistic flame-retardant EP-TPV composite material comprises the following raw materials in parts by weight:
ethylene Propylene Diene Monomer (EPDM) 26.4 parts
39.6 Portions of Polypropylene (PP)
Pentaerythritol (PER) 12.68 parts
12.32 portions of Melamine Phosphate (MP)
9 portions of Zinc Borate (ZB)
The material selection type is the same as that of the example (1);
a preparation method of a halogen-free synergistic flame-retardant modified EP-TPV material comprises the following steps:
(1) the EPDM was placed at 70oC, drying in a constant-temperature drying oven for 8 hours, and then filling oil (naphthenic oil with 30 percent of rubber content) for 24 hours at room temperature; PP was also placed at 70oC, drying in a constant-temperature drying box for 8 hours;
(2) placing 26.4 parts of EPDM, 14.6 parts of PP and DCP crosslinking agent with the rubber content of 1.2wt% in a double-screw extruder for extrusion processing to prepare the EP-TPV matrix, wherein the rotating speed of a main machine screw is 250r/min, and the processing temperature is 185-oC；
(3) Placing MP, PER, ZB and PP at 70oC, drying in a constant-temperature drying box for 8 hours; placing MP, PER, ZB and PP at 70oC, drying in a constant-temperature drying box for 8 hours; then uniformly mixing PER12.68 parts, MP12.32 parts, ZB9 parts and PP25 parts, performing reaction extrusion to prepare the flame-retardant master batch, and controlling the processing temperature to 260-oC, the rotating speed of the screw is 200 r/min;
(4) uniformly mixing the EP-TPV matrix in the step (2) and the synergistic flame-retardant master batch in the step (3) according to a formula ratio, extruding and granulating the mixture by a double-screw extruder to prepare halogen-free synergistic flame-retardant EP-TPV granules, wherein the rotating speed of a main machine screw is higher than that of a main machine screw250r/min, processing temperature 185-oC。
The test of mechanical properties, namely the tensile property test, the specification of the dumbbell-shaped test sample is 75 × (5 +/-0.1) × (2 +/-0.1) mm, the initial position of a clamp is 52mm, the gauge length is 25mm, and the specification is 23 +/-2oAnd C, testing according to an ASTM D638-10 standard, wherein the tensile speed is 50mm/min, and 1 group of 5 bars are tested and averaged.
The bending property test shows that the specification of the rod-shaped test sample is 64 × (10 +/-0.1) × (4 +/-0.1) mm, the span is 52mm, and the bending property is 23 +/-2oAnd C, testing according to an ASTM D790-10 standard, wherein the bending speed is 2mm/min, and 1 group of 5 bars are tested to obtain an average value.
Limiting oxygen index test: and (3) performing a Limiting Oxygen Index (LOI) test by adopting a JF-3 type oxygen index tester according to GB/T2406.2-2009 standard, wherein each group of samples is tested for 5 times, and the sample size is 80 +/-2 mm multiplied by 10 +/-0.2 mm multiplied by 4 +/-0.2 mm.
UL-94 burning grade test: the test was carried out on a vertical burner type SH5300 according to GB/T5169.16-2008, each set of samples being tested 5 times with sample sizes of 125. + -. 4 mm X13.0. + -. 0.2mm X3.0. + -. 0.3 mm.
The mechanical and flame retardant properties test results for examples 1-5 are shown in table 1 below:
TABLE 1
| Test items | Existing EP-TPV | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| Tensile Strength (MPa) | 20.45±0.40 | 25.6 | 22.3 | 20.5 | 18.2 | 16.4 |
| Flexural Strength (MPa) | 8.5 | 22.9 | 23.6 | 23.9 | 25.1 | 26.7 |
| Elongation at Break (%) | 555 | 432 | 395 | 347 | 305 | 162 |
| Limiting oxygen index | 18.5 | 27.2 | 28.3 | 29.4 | 29.8 | 30.1 |
| UL-94 vertical burning rating | Grade free | Class V-1 | Class V-0 | Class V-0 | Class V-0 | Class V-0 |
| Initial thermal degradation temperature (oC） | 273.0 | 397.6 | 407.5 | 410.9 | 416.4 | 417.5 |
As can be seen from Table 1, the halogen-free synergistic flame-retardant EP-TPV material can slightly improve the rigidity of the composite material on the basis of obviously improving the flame-retardant performance, keeps the elastomer characteristic of the material to a greater extent, and has better processability and excellent comprehensive performance.
The halogen-free synergistic flame-retardant EP-TPV material disclosed by the invention is extruded to generate pentaerythritol phosphate melamine salt containing (P = O) -O-C structure through the reaction of MP and PER in the processing process, the flame retardant property of the composite material is obviously improved due to the synergistic effect of the structure and zinc borate, the UL-94 vertical combustion grade is improved from no grade to V-0 grade, and the oxygen index can reach 30.
The above-described embodiments are preferred implementations of the present invention, and the present invention may be implemented in other ways without departing from the spirit of the present invention.
Claims (3)
1. A halogen-free synergistic flame-retardant EP-TPV composite material is characterized in that: calculated according to the mass portion, comprises 26.4 to 28.8 portions of ethylene propylene diene monomer; 39.6-43.2 Parts of Polypropylene (PP); 25 parts of a reactive halogen-free flame retardant; 3-9 parts of a synergist.
2. The halogen-free synergistic flame retardant EP-TPV composite according to claim 1, characterized in that: the 25 parts of the reactive halogen-free flame retardant respectively comprise 12.68 parts of Pentaerythritol (PER) and 12.32 parts of Melamine Phosphate (MP); the synergist is zinc borate.
3. The preparation method of the microcellular ethylene propylene diene monomer material with high foaming ratio as claimed in claim 1, which is characterized in that: (1) uniformly mixing PER12.68 parts, MP12.32 parts, ZB3-9 parts and PP25 parts, carrying out reactive extrusion in a double-screw extruder, and controlling the processing temperature to 260-oC, preparing the synergistic flame-retardant master batch at the screw rotating speed of 200 r/min; (2) uniformly mixing the synergistic flame-retardant master batch in the step (1) with an EP-TPV matrix (containing 26.4-28.8 parts of EPDM and 14.6-18.2 parts of PP), extruding and granulating by a double-screw extruder, and finally controlling the rubber-plastic ratio in the composite material to be 40/60 (containing 26.4-28.8 parts of EPDM and 39.6-43.2 parts of PP), the content of the reactive flame retardant to be 25 percent and the content of the synergistic agent to be 3-9 percent; the rotation speed of the screw of the host machine is 250r/min, and the processing temperature is 185-oAnd C, after shearing and mixing by an extruder, melting and compounding the materials, finally extruding, cooling and granulating to obtain a finished product.
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| CN114874555A (en) * | 2022-04-15 | 2022-08-09 | 贵州省材料技术创新基地 | Low-friction coefficient dynamic sealing rubber composite material and preparation method thereof |
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