CN111205623A - Double-base synergistic flame-retardant polyphenyl ether composite material and preparation method thereof - Google Patents
Double-base synergistic flame-retardant polyphenyl ether composite material and preparation method thereof Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
- C08L71/08—Polyethers derived from hydroxy compounds or from their metallic derivatives
- C08L71/10—Polyethers derived from hydroxy compounds or from their metallic derivatives from phenols
- C08L71/12—Polyphenylene oxides
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- C08L2201/02—Flame or fire retardant/resistant
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
Abstract
The invention discloses a double-base synergistic flame-retardant polyphenyl ether composite material which comprises, by mass, 80-95 parts of polyphenyl ether, 2-5 parts of a gas-phase flame retardant, 2-5 parts of a condensed-phase flame retardant, 5-10 parts of a compatibilizer and 0.5 part of an antioxidant. The method comprises the following steps: s1, drying the polyphenyl ether, the gas-phase flame retardant, the condensed-phase flame retardant, the compatibilizer and the antioxidant at 75-85 ℃, and mixing uniformly to obtain a mixture; s2, subjecting the mixture obtained in the step S1 to blending extrusion processing through a double-screw extruder at 290-305 ℃, then cooling to room temperature, and then sequentially carrying out traction and grain cutting to obtain the phosphaphenanthrene and polyphosphazene double-base synergistic flame-retardant polyphenyl ether composite material. The modified polyphenyl ether material has good flame retardant property, good compatibility of the flame retardant and a matrix, and good mechanical property; in addition, the preparation method is simple.
Description
Technical Field
The invention belongs to the field of polyphenyl ether composite materials, and particularly relates to a phosphaphenanthrene and polyphosphazene double-base synergistic flame-retardant polyphenyl ether composite material and a preparation method thereof.
Background
Polyphenylene oxide (PPO for short in English) is mainly used in the aspects of electronic appliances, automobiles, household appliances, office equipment, industrial machinery and the like, and is used for manufacturing automobile instrument panels, radiator grids, loudspeaker grids, consoles, fuse boxes, relay boxes, connectors and wheel covers by utilizing the heat resistance, impact resistance, dimensional stability, scratch resistance, stripping resistance, coatability and electrical performance of MPPO; the electronic and electrical industry is widely used for manufacturing parts such as connectors, coil bobbins, switching relays, tuning devices, large-scale electronic displays, variable capacitors, storage battery accessories, microphones and the like. The household appliances are used for parts such as televisions, video cameras, video tapes, recorders, air conditioners, heaters, electric cookers and the like. Polyphenylene ethers, however, are readily combustible. The halogen-containing flame retardant is applied to polyphenyl ether resin and mainly comprises polybrominated biphenyl compounds, and the halogen-containing flame retardant has good flame retardant effect on polyphenyl ether materials, but can emit toxic and corrosive gases and smoke during combustion or high-temperature processing. Environmental pollution and harm to human health are caused, WEEE and RoHS are published in European Union 2003, the requirements of people on the quality of environmental life are higher and higher, and various national environment-friendly documents are continuously provided, so that the trend of the high-molecular flame-retardant material is mainly halogen-free.
Among many halogen-free flame retardants, phosphorus-based flame retardants have been the focus of research in the field of flame retardancy. The phosphaphenanthrene-containing compound 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and derivatives thereof and 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-sulfide (DOPS) and derivatives thereof are novel flame retardants, have excellent flame retardant properties and are widely used for polymer-based halogen-free flame retardant composite materials. Compared with common acyclic organic phosphate, the phosphaphenanthrene has better thermal stability and chemical stability, and also has the advantages of low phosphorus content, no halogen, low smoke, no toxicity, no migration, durable flame retardance and the like.
However, the DOPO flame retardant has the defects that the compatibility between the flame retardant and the polymer matrix or the reinforced material is poor, so that the mechanical property of the polymer matrix or the reinforced material is reduced when the flame retardant is used.
Disclosure of Invention
In order to solve the technical problems, the invention provides a double-base synergistic flame-retardant polyphenyl ether composite material and a preparation method thereof. The modified polyphenyl ether material has good flame retardant property, good compatibility of the flame retardant and a matrix, and good mechanical property; in addition, the preparation method is simple.
The technical scheme adopted by the invention is as follows:
the invention provides a double-base synergistic flame-retardant polyphenyl ether composite material which comprises, by mass, 80-95 parts of polyphenyl ether, 2-5 parts of gas-phase flame retardant, 2-5 parts of condensed-phase flame retardant, 5-10 parts of compatibilizer and 0.5 part of antioxidant.
Preferably, the composite material comprises 90 parts by mass of polyphenylene ether, 2.5 parts by mass of gas-phase flame retardant, 2.5 parts by mass of condensed-phase flame retardant, 5 parts by mass of compatibilizer and 0.5 part by mass of antioxidant.
The formula of the invention has the beneficial effects that: due to the synergistic effect of the gas-phase flame retardant and the condensed-phase flame retardant, the gas-phase flame retardant mainly acts on gas-phase flame retardance, and the condensed-phase flame retardant is weaker in flame retardance. The condensed phase flame retardant takes condensed phase action as a principal and subordinate action to make up for the mixing of the gas-phase flame retardant, the liquid-phase flame retardant and the polyphenyl ether, so that the flame retardant has more excellent flame retardant performance and excellent interface compatibility, and the mechanical property of the polymer flame retardant material is not reduced and is enhanced. Due to the addition of the compatibilizer and the antioxidant, more excellent mechanical properties are obtained. Solves the technical problem that the compatibility between the DOPO flame retardant and the polymer matrix or the reinforced material in the background technology is poor, so that the mechanical property of the flame retardant is reduced when the flame retardant is used.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, the gas-phase flame retardant is reactive phosphaphenanthrene.
The reaction type phosphaphenanthrene has good gas-phase flame retardant effect. And the hydroxyl reaction group can be matched with polyphenyl ether to form better flame retardant effect.
Further, the reactive phosphaphenanthrene is any one of DOPO-HQ, DOPS-HQ, DOPO-PHBA, DOPS-PHBA, (DOPO)2-P-PPD-PH or (DOPS)2-P-PPD-PH, wherein: the structural formulas of DOPO-HQ, DOPS-HQ, DOPO-PHBA, DOPS-PHBA, (DOPO)2-P-PPD-PH and (DOPS)2-P-PPD-PH are respectively as follows:
further, the condensed phase flame retardant is a reactive polyphosphazene, wherein the reactive polyphosphazene has the following structural formula:
further, the compatibilizer is any one of polyethylene grafted glycidyl methacrylate, glycidyl methacrylate grafted ethylene-octene copolymer, ethylene-butyl acrylate-glycidyl methacrylate terpolymer or styrene-acrylonitrile grafted glycidyl methacrylate.
Further, the antioxidant is bis (2, 4-dicumylphenyl) pentaerythritol diphosphite.
Compared with the prior art, the invention has the following beneficial effects:
1. all the reactive phosphaphenanthrene flame retardants and reactive polyphosphazenes have hydroxyl reactive groups, a compatibilizer with epoxy active groups is added, the epoxy active groups can react with the reactive phosphaphenanthrene flame retardants, the reactive polyphosphazenes and polyphenylene ether matrix resins to generate a cross-linked network structure, and the interface structures between the reactive phosphaphenanthrene flame retardants and the polyphenylene ether matrix resins, between the reactive phosphaphenanthrene flame retardants and the reactive polyphosphazenes and between the reactive polyphosphazenes and the polyphenylene ether matrix resins are enhanced, so that the flame retardant property and the interface bonding force of the reactive phosphaphenanthrene flame retardants and the reactive polyphosphazenes to the polyphenylene ether matrix resins are enhanced, the mechanical property is not reduced due to the addition of the flame retardants, and the mechanical property of the polyphenylene ether flame-retardant composite material is also improved.
2. The reactive phosphaphenanthrene flame retardant and the reactive polyphosphazene generate double-base synergistic action of gas-phase flame retardance and condensed-phase flame retardance in polyphenyl ether matrix resin, so that the flame retardance of the reactive phosphaphenanthrene flame retardant is mainly gas-phase flame retardance. The reactive polyphosphazene is mainly used for coacervate phase flame retardant action, the reactive phosphaphenanthrene flame retardant and the reactive polyphosphazene are subjected to synergistic flame retardant action, the gas phase flame retardant action of the phosphaphenanthrene is achieved, the polyphosphazene is also used for enhancing the coacervate phase flame retardant action, in the combustion process, not only the oxygen content of gases generated during the combustion of the phosphaphenanthrene is reduced, but also the phosphoric acid generated during the combustion of the phosphaphenanthrene promotes the carbonization action.
3. The char forming capability of the material is stronger in the combustion process of the polyphosphazene, and in addition, the reactive phosphaphenanthrene and the polyphosphazene also have the nitrogen-phosphorus-sulfur triple-element synergistic flame retardant effect, so that the reactive phosphaphenanthrene and the polyphosphazene generate a double-base synergistic flame retardant effect and a nitrogen-phosphorus-sulfur triple-element synergistic flame retardant effect, and the material has more excellent flame retardant property. The invention has wide material source, easy acquisition and good use effect.
The invention also provides a preparation method of the double-base synergistic flame-retardant polyphenyl ether composite material, which comprises the following steps:
s1, drying the polyphenyl ether, the gas-phase flame retardant, the condensed-phase flame retardant, the compatibilizer and the antioxidant at 75-85 ℃, and mixing uniformly to obtain a mixture;
s2, subjecting the mixture obtained in the step S1 to blending extrusion processing through a double-screw extruder at 290-305 ℃, then cooling to room temperature, and then sequentially carrying out traction and grain cutting to obtain the phosphaphenanthrene and polyphosphazene double-base synergistic flame-retardant polyphenyl ether composite material.
The invention has the beneficial effects that the existing double-screw extruder is adopted, and the existing extrusion process is used for processing, traction and grain cutting. The particle material of the phosphaphenanthrene and polyphosphazene double-base synergistic flame-retardant polyphenyl ether composite material can also be dried and then injection-molded into a standard sample strip for testing.
Detailed Description
The principles and features of this invention are described below in conjunction with examples which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
Example 1
A preparation method of a double-base synergistic flame-retardant polyphenyl ether composite material comprises the following steps:
s1, drying 90kg of polyphenyl ether, 2.5kg of reactive phosphaphenanthrene, 2.5kg of reactive polyphosphazene, 5kg of styrene-acrylonitrile grafted glycidyl methacrylate and 0.5kg of bis (2, 4-dicumylphenyl) pentaerythritol diphosphite at 80 ℃, and mixing uniformly to obtain a mixture. Drying for 1-4 hr until no water is apparent.
S2, blending and extruding the mixture obtained in the step S1 at 290-305 ℃ through a double-screw extruder, cooling to room temperature, and then sequentially drawing and granulating to obtain the polylactic acid, phosphaphenanthrene and polyphosphazene double-base synergistic flame-retardant composite material.
The structure of the reactive phosphaphenanthrene is shown below.
Example 2
The difference from example 1 is that 1.5kg of the gas-phase flame retardant and 1.5kg of the condensed-phase flame retardant were used in step S1.
Comparative example 1
The difference from example 1 is that: in step S1, 90kg of polyphenylene ether, 5kg of a gas phase flame retardant, 5kg of a compatibilizer, and 0.5kg of an antioxidant were dried at 80 ℃ and mixed to obtain a mixture. No coacervate phase flame retardant was added.
Comparative example 2
The difference from example 1 is that: in step S1, 90kg of polyphenylene ether, 5kg of condensed phase flame retardant, 5kg of compatibilizer, and 0.5kg of antioxidant were dried at 80 ℃ and mixed to obtain a mixture. No gas phase flame retardant was added.
The effect proves experiment: the phosphaphenanthrene and polyphosphazene double-base synergistic flame-retardant polyphenylene oxide composite materials obtained in the above example 1, example 2, comparative example 1 and comparative example 2 are all injected into standard sample bars for the following tests:
vertical burning performance: the test was carried out according to the vertical method of GB/T2408-1996, with at least 5 standard bars per set, i.e., 5 bars for example 1, example 2, comparative example 1 and comparative example 2.
The flame retardant grade, namely the property of the substance or the treated material for obviously delaying the flame spread, is classified according to a grading system, and the flame retardant grade is gradually increased from V2 to V1 to V0: v0 shows that after the sample is subjected to two 10-second combustion tests, the flame is extinguished within 30 seconds, and no combustible can fall off; v1 shows that after the sample is subjected to two 10-second combustion tests, the flame is extinguished within 60 seconds, and no combustible can fall off, and V2 shows that after the sample is subjected to two 10-second combustion tests, the flame is extinguished within 60 seconds, and the combustible can fall off.
Testing of mechanical properties: each group of test sample strips is 10, and the result is the average value of 10 test values; the tensile strength is tested according to GB/T1040-2006, and the bending strength is tested according to GB/T9341-2000;
the notch impact strength was notched by 4mm using a notch sampling machine and tested in accordance with GB/T1043-2008.
The results of the performance tests obtained above are shown in table 1:
TABLE 1 composite Performance test
| Test items | Example 1 | Example 2 | Comparative example 1 | Comparative example 2 |
| Tensile Strength (MPa) | 47.8 | 42.3 | 37.6 | 36.5 |
| Flexural Strength (MPa) | 68.6 | 61.4 | 58.7 | 57.4 |
| Notched Izod impact Strength (KJ/m)2) | 13.7 | 12.6 | 10.3 | 10.6 |
| Flame retardant rating (UL94) | V0 | V0 | V2 | V2 |
| Surface quality | Without pattern | Without pattern | Without pattern | Without pattern |
| Degree of difficulty of molding | Is easy to use | Is easy to use | Is easy to use | Is easy to use |
Compared with the conventional material, the mechanical property of the general polymer-based flame-retardant material is reduced along with the increase of the content of the flame retardant in the sample prepared by the technical scheme of the invention, and the difference between the example 1 and the example 2 in the invention is as follows: the amount of the reactive phosphaphenanthrene flame retardant used in example 1 was 2.5kg, the amount of the reactive polyphosphazene used was 2.5kg, and the amount of the reactive phosphaphenanthrene flame retardant used in example 2 was 1.5kg, the amount of the reactive polyphosphazene used was 1.5kg, and the other experimental conditions were the same. In the examples 1 and 2, it can be seen that, by adopting the reactive phosphaphenanthrene flame retardant and the reactive polyphosphazene, the content of the flame retardant is increased, not only the mechanical properties of the polyphenylene ether flame-retardant composite material are not reduced, but also the mechanical properties of the polyphenylene ether flame-retardant composite material are increased, because the reactive hydroxyl group in the reactive phosphaphenanthrene flame retardant, the reactive hydroxyl group in the reactive polyphosphazene and the reactive hydroxyl group in the polyphenylene ether matrix resin can react with the epoxy group in the ethylene-butyl acrylate-glycidyl methacrylate terpolymer compatibilizer, the interfacial adhesion between the reactive phosphaphenanthrene flame retardant and the reactive polyphosphazene is enhanced, the interfacial adhesion between the reactive phosphaphenanthrene flame retardant and the polyphenylene ether matrix is increased, and the interfacial strength between the reactive polyphosphazene and the polyphenylene ether matrix is enhanced, the polyphenyl ether flame-retardant composite material forms a network cross-linking structure, and the mechanical property of the polyphenyl ether flame-retardant composite material is better along with the increase of the dosage of the reactive phosphaphenanthrene and the reactive polyphosphazene, so that the reactive phosphaphenanthrene and the reactive polyphosphazene have the flame retardant effect in the polyphenyl ether flame-retardant composite material and have the function of interface compatibilization; the two polyphenylene ether flame retardant composites of example 1 and example 2 were rated V0, except that the difference in the amounts of reactive phosphaphenanthrene and reactive polyphosphazene resulted in the difference in mechanical properties of the polyphenylene ether flame retardant composites. The difference between the example 1 and the comparative examples 1 and 2 is that the addition amount of the reactive phosphaphenanthrene and the reactive polyphosphazene in the raw material formula of the comparative example 1 is 2.5kg, the sum of the flame retardants is 5kg, the addition amount of the reactive phosphaphenanthrene and the reactive polyphosphazene in the raw material formula of the comparative example 1 is only 5kg, the addition amount of the reactive polyphosphazene in the raw material formula of the comparative example 2 is only 5kg, and the other experimental raw materials and conditions are the same, as shown in the table 1, the flame retardant grades of the polyphenyl ether flame retardant composite materials of the comparative examples 1 and 2 are both V2 grades, and the flame retardant grade of the polyphenyl ether flame retardant composite material of the example 1 is both V0 grades, which shows that the flame retardant effect of the polyphenyl ether composite materials with the reactive phosphaphenanthrene and the reactive polyphosphazene added separately is poor because only gas phase or condensed phase is mainly, in the embodiment 1, the reactive phosphaphenanthrene and the reactive polyphosphazene are added, so that the polyphenyl ether flame-retardant composite material has gas-phase and condensed-phase double-base synergistic flame retardance and excellent nitrogen-phosphorus-sulfur synergistic flame retardance, and the polyphenyl ether flame-retardant composite material in the embodiment 1 has excellent flame retardance. In addition, example 2 is different from the polyphenylene ether flame retardant composite materials of comparative examples 1 and 2 in that: the dosage of the reactive phosphaphenanthrene flame retardant in the embodiment 2 is 1.5kg, the dosage of the reactive polyphosphazene is 1.5kg, and the sum of the flame retardants is 3kg, while the raw material formula in the comparative example 1 only adds 5kg of reactive phosphaphenanthrene, the raw material formula in the comparative example 2 only adds 5kg of reactive polyphosphazene, the rest experimental raw materials and conditions are the same, the flame retardant grade of the polyphenylene ether flame-retardant composite material which is 3kg of the flame retardant in the example 2 is V0 grade, while the flame retardant rating of the polyphenylene ether flame retardant composite material of comparative example 1 and comparative example 2 having a flame retardant amount of 5kg was only V2, thus indicating that the reactive phosphaphenanthrene and the reactive polyphosphazene have excellent double-base synergistic effect and nitrogen-phosphorus-sulfur triple-element synergistic flame-retardant effect, therefore, the polyphenyl ether flame-retardant composite material with lower content of the reactive phosphaphenanthrene and the reactive polyphosphazene is added to obtain excellent flame-retardant property.
Example 3
A preparation method of a double-base synergistic flame-retardant polyphenyl ether composite material comprises the following steps:
s1, drying 80kg of the polyphenyl ether, 2kg of reactive phosphaphenanthrene, 2kg of reactive polyphosphazene, 5kg of polyethylene grafted glycidyl methacrylate and 0.5kg of bis (2, 4-dicumylphenyl) pentaerythritol diphosphite at 75 ℃, and mixing uniformly to obtain a mixture. Drying for 1-4 hr until no water is apparent.
S2, blending and extruding the mixture obtained in the step S1 at 290-305 ℃ through a double-screw extruder, cooling to room temperature, and then sequentially drawing and granulating to obtain the polylactic acid, phosphaphenanthrene and polyphosphazene double-base synergistic flame-retardant composite material.
The structure of the reactive phosphaphenanthrene is shown below.
Example 4
A preparation method of a double-base synergistic flame-retardant polyphenyl ether composite material comprises the following steps:
s1, drying 95kg of polyphenyl ether, 5kg of reactive phosphaphenanthrene, 5kg of reactive polyphosphazene, 10kg of ethylene-butyl acrylate-glycidyl methacrylate terpolymer and 0.5kg of bis (2, 4-dicumylphenyl) pentaerythritol diphosphite at 85 ℃, and mixing uniformly to obtain a mixture. Drying for 1-4 hr until no water is apparent.
S2, blending and extruding the mixture obtained in the step S1 at 290-305 ℃ through a double-screw extruder, cooling to room temperature, and then sequentially drawing and granulating to obtain the polylactic acid, phosphaphenanthrene and polyphosphazene double-base synergistic flame-retardant composite material.
The structure of the reactive phosphaphenanthrene is shown below.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. A double-base synergistic flame-retardant polyphenyl ether composite material is characterized in that: the flame retardant comprises, by mass, 80-95 parts of polyphenylene oxide, 2-5 parts of a gas-phase flame retardant, 2-5 parts of a condensed-phase flame retardant, 5-10 parts of a compatibilizer and 0.5 part of an antioxidant.
2. The bis-based synergistic flame retardant polyphenylene ether composite material according to claim 1, wherein: the composite material comprises, by mass, 90 parts of polyphenylene oxide, 2.5 parts of a gas-phase flame retardant, 2.5 parts of a condensed-phase flame retardant, 5 parts of a compatibilizer and 0.5 part of an antioxidant.
3. The bis-based synergistic flame retardant polyphenylene ether composite material according to claim 1, wherein: the gas-phase flame retardant is reactive phosphaphenanthrene.
4. The bis-based synergistic flame retardant polyphenylene ether composite material according to claim 3, wherein: the reactive phosphaphenanthrene is any one of DOPO-HQ, DOPS-HQ, DOPO-PHBA, DOPS-PHBA, (DOPO)2-P-PPD-PH or (DOPS)2-P-PPD-PH, wherein: the structural formulas of DOPO-HQ, DOPS-HQ, DOPO-PHBA, DOPS-PHBA, (DOPO)2-P-PPD-PH and (DOPS)2-P-PPD-PH are respectively as follows:
5. the bis-based synergistic flame retardant polyphenylene ether composite material according to claim 1, wherein: the condensed phase flame retardant is reactive polyphosphazene.
6. The bis-based synergistic flame retardant polyphenylene ether composite material according to claim 5, wherein: the structural formula of the reactive polyphosphazene is as follows:
7. the bis-based synergistic flame retardant polyphenylene ether composite material according to claim 1, wherein: the compatibilizer is any one of polyethylene grafted glycidyl methacrylate, glycidyl methacrylate grafted ethylene-octene copolymer, ethylene-butyl acrylate-glycidyl methacrylate terpolymer or styrene-acrylonitrile grafted glycidyl methacrylate.
8. The bis-based synergistic flame retardant polyphenylene ether composite material according to claim 1, wherein: the antioxidant is bis (2, 4-dicumylphenyl) pentaerythritol diphosphite.
9. A method for preparing a double-base synergistic flame-retardant polyphenylene ether composite material according to any one of claims 1 to 8, which comprises the following steps:
s1, drying the polyphenyl ether, the gas-phase flame retardant, the condensed-phase flame retardant, the compatibilizer and the antioxidant at 75-85 ℃, and mixing uniformly to obtain a mixture;
s2, subjecting the mixture obtained in the step S1 to blending extrusion processing through a double-screw extruder at 290-305 ℃, then cooling to room temperature, and then sequentially carrying out traction and grain cutting to obtain the phosphaphenanthrene and polyphosphazene double-base synergistic flame-retardant polyphenyl ether composite material.
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| CN113461895A (en) * | 2021-06-17 | 2021-10-01 | 淮阴工学院 | Preparation method of organosilane modified hyperbranched polyphenyl ether |
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