CN115260756A - Halogen-free flame-retardant bio-based high-temperature-resistant nylon alloy/polyphenyl ether composite material - Google Patents
Halogen-free flame-retardant bio-based high-temperature-resistant nylon alloy/polyphenyl ether composite materialDownload PDFInfo
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- CN115260756A CN115260756ACN202210965040.4ACN202210965040ACN115260756ACN 115260756 ACN115260756 ACN 115260756ACN 202210965040 ACN202210965040 ACN 202210965040ACN 115260756 ACN115260756 ACN 115260756A
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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
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
- 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
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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Abstract
Description
Technical Field
The invention belongs to the technical field of plastics, and particularly relates to a halogen-free flame-retardant bio-based high-temperature-resistant nylon alloy/polyphenyl ether composite material.
Background
Nylon and polyphenylene ether are high-performance resin materials, and alloys containing both are also being studied. The prior art discloses a halogen-free flame-retardant polyphenyl ether composition with high CTI (comparative tracking index), a preparation method and application thereof, wherein the halogen-free flame-retardant polyphenyl ether composition comprises the following components: 60-80 parts of polyphenyl ether, 10-20 parts of polystyrene resin, 2-10 parts of toughening agent, 5-15 parts of organic phosphorus flame retardant, 0.5-1.5 parts of linear low density polyethylene, 1-6 parts of magnesium hydroxide, 1-4 parts of nylon and 0.2-1 part of antioxidant; can reach 0-level CTI and has good silica gel bonding performance. The prior art discloses a nylon-polyphenylene oxide composite material and a preparation method thereof, wherein the nylon-polyphenylene oxide composite material is prepared by mixing and injection molding a first component of 90-99.9wt% and a second component of 0.1-10wt%, wherein: the first component is prepared by mixing and extruding 30-80wt% of nylon, 20-65wt% of polyphenyl ether, 1-10wt% of chain extender and 0.05-2wt% of antioxidant; the second component is a hollow microsphere foaming agent; the technology uses the hollow microsphere foaming agent as the foaming agent, so that the apparent quality of the PA/PPO composite material can be improved, and the chain extender is beneficial to improving the compatibility and the melt strength of the material and improving the foaming effect of the foaming agent, so that the apparent quality of the composite material is further improved. The prior art discloses a polyphenyl ether and nylon composition and a preparation method thereof, and the composition comprises the following components in percentage by weight: 20 to 50 percent of polyphenyl ether, 27 to 70 percent of nylon, 0 to 50 percent of glass fiber and 2 to 6 percent of liquid polybutadiene; the technology uses liquid polybutadiene to carry out blending modification in polyphenyl ether and nylon, toughens the polyphenyl ether and nylon, improves the hydrolysis resistance of the polyphenyl ether, and can keep the heat resistance and the flame retardance of the polyphenyl ether not to be reduced, thereby not limiting the temperature application range of the modified polyphenyl ether. In the prior art, MXD6, bio-based nylon, polyphenyl ether, compatilizer, antioxidant, lubricant, coupling agent and oil-soluble nigrosine are weighed and added into a high-speed stirrer for blending and stirring; then adding the materials into a double-screw extruder, heating to 235-275 ℃ to melt the mixture; adding glass fiber into a double-screw extruder according to a proportion, and blending and extruding the glass fiber and the material into strips; cooling the extruded material, and then pelletizing and drying the material to obtain a finished product; the technology improves the temperature resistance by using MXD 6. In the prior art, few reports are made on preparing the flame-retardant composite material mainly from bio-based nylon.
Disclosure of Invention
The invention discloses a halogen-free flame-retardant bio-based high-temperature-resistant nylon alloy/polyphenyl ether composite material, which takes bio-based nylon and polyphenyl ether as main bodies and combines conventional auxiliaries to obtain the composite material with excellent flame retardant performance and heat resistance, good alcohol resistance and electrical performance and further reduced moisture absorption rate of the material.
The invention adopts the following technical scheme:
a halogen-free flame-retardant bio-based high-temperature-resistant nylon alloy/polyphenyl ether composite material comprises PA56, PA10T, polyphenyl ether, a flame retardant, a toughening agent, a nucleating agent, an antioxidant and a lubricant; preferably, the halogen-free flame-retardant bio-based high-temperature-resistant nylon alloy/polyphenyl ether composite material is prepared from PA56, PA10T, polyphenyl ether, a flame retardant, a toughening agent, a nucleating agent, an antioxidant and a lubricant.
In the invention, the mass percentages of PA56, PA10T, polyphenyl ether, flame retardant, toughening agent, nucleating agent, antioxidant and lubricant are respectively 10-20%, 20-50%, 10-30%, 10-20%, 5-10%, 1-3%, 0-1% and 0-1%; preferably 10-20%, 30-40%, 15-25%, 15-20%, 5-10%, 1-3%, 0.3-0.8%, 0.3-0.7%; the total amount is 100%.
In the invention, the flame retardant is one or more of organic hypophosphite, inorganic hypophosphite, melamine salt, polyphosphate and fluorine-containing anti-dripping agent; the toughening agent is one or more of maleic anhydride grafted styrene-butadiene-styrene copolymer, maleic anhydride grafted hydrogenated styrene-butadiene-styrene copolymer, hydrogenated styrene-butadiene-styrene copolymer and styrene-ethylene-propylene double-block polymer; the nucleating agent is one or more of long-chain saturated linear carboxylate, sorbitol compound, nonanol compound, xylitol compound, phosphorus compound and triaminobenzene derivative; the antioxidant comprises copper salt antioxidant, hindered phenol antioxidant, hindered amine antioxidant, phosphite antioxidant, phosphate antioxidant, and epoxy resin antioxidant; the lubricant is a silicon-based lubricant or an amide-based lubricant.
The invention discloses a preparation method of the halogen-free flame-retardant bio-based high-temperature-resistant nylon alloy/polyphenyl ether composite material, which comprises the steps of melting and mixing PA56, PA10T, polyphenyl ether, a flame retardant, a toughening agent, a nucleating agent, an antioxidant and a lubricant to obtain the halogen-free flame-retardant bio-based high-temperature-resistant nylon alloy/polyphenyl ether composite material; as a general knowledge, a screw extruder may be used for the raw material mixing.
The invention discloses an application of the halogen-free flame-retardant bio-based high-temperature-resistant nylon alloy/polyphenyl ether composite material in preparation of flame-retardant plastics.
The invention mainly uses the bio-based nylon material and the polyphenyl ether, improves the heat resistance, the flame retardance, the electrical property and the alcohol resistance of the whole alloy material due to different formula designs, reduces the moisture absorption of the material, reduces emission and protects the environment. The combination of the three main resins and the selection of the auxiliary agent not only improve the heat resistance of nylon, but also reduce the moisture absorption rate and improve the processability, and the flame retardant is used to realize the flame retardant property, and particularly, the flame retardant is added into a resin matrix to jointly improve the flame retardant property of the composite material.
The halogen-free flame-retardant alloy material can improve the combustibility of non-flame-retardant materials, achieves the UL94-V0 combustion grade, particularly can be made to be 0.4mm-V0, and especially improves the combustibility of PA56/PA 10T; the alloy material has higher thermal performance (thermal deformation can reach 150 ℃); the alloy material can improve the overall alcohol resistance, can pass a 135 ℃/1000H test and has the performance retention rate of over 90 percent; the alloy material reduces the moisture absorption rate of the conventional alloy material (most of PPO/PA), improves the dimensional stability, and particularly improves the moisture absorption of PA56 with higher moisture absorption; the alloy material has low dielectric constant and relative tracking index of over 600V.
Detailed Description
The preparation method comprises the following steps of melting and mixing PA56, PA10T, polyphenyl ether, a flame retardant, a toughening agent, a nucleating agent, an antioxidant and a lubricant to obtain a halogen-free flame-retardant bio-based high-temperature-resistant nylon alloy/polyphenyl ether composite material; as a general knowledge, a screw extruder may be used for the raw material mixing. Concretely, adding bio-based nylon (PA 56, PA 10T), polyphenyl ether and a toughening agent into a mixer, and mixing for 10-15 min to obtain a premix; adding the nucleating agent, the antioxidant and the lubricant into a mixer, and mixing for 3-5 min to obtain an additive premix; adding the two obtained premix compounds into a main feeding and discharging barrel of a double-screw extruder, feeding the flame retardant into the double-screw extruder from the side direction of the extruder, and performing melt extrusion and granulation to obtain the halogen-free flame-retardant bio-based nylon/polyphenyl ether composite material; the extrusion temperature of the extruder is 220-280 ℃, the screw rotation speed is 200-500 rpm, and the temperature of each section is conventional technology.
The raw materials used in the invention are commercially available products, which meet the conventional requirements of PA and PPO alloy preparation, such as PA10T and H101 new materials; PPO, LXR40C blue star new chemical material; PA56, kessentian E1273; flame retardant, organic aluminum hypophosphite, claino OP1240. The specific preparation operation and the test method are conventional techniques.
Examples
Adding bio-based nylon (PA 56, PA 10T), polyphenyl ether and a toughening agent into a mixer according to the formula shown in the table 1, and mixing for 10min to obtain a premix; adding the nucleating agent, the antioxidant and the lubricant into a mixer, and mixing for 5min to obtain an additive premix; adding the two obtained premix compounds into a main feeding and discharging barrel of a double-screw extruder, feeding the flame retardant into the discharging barrel through the side direction of the extruder, feeding the flame retardant into the double-screw extruder, and performing melt extrusion and granulation to obtain the halogen-free flame-retardant bio-based nylon/polyphenyl ether composite material; the extrusion temperature of the extruder is 220-280 ℃, and the screw rotating speed is 300rpm.
Performance characterization
Flame retardance: UL94 0.4mm. The flame retardance of the halogen-free flame-retardant bio-based nylon/polyphenylene oxide composite material reaches V0, the third comparative example is V1, and the fourth comparative example is HB.
Heat distortion temperature: ISO 75.80MPa. Example one is 150 ℃ and the test is 147.5 ℃ after soaking in ethylene glycol aqueous solution at high temperature (135 ℃/1000H).
Tensile strength (before and after high-temperature soaking in ethylene glycol aqueous solution, 135 ℃/1000H): ISO 527. The retention after soaking of the first example was 92%. The retention rate after soaking of the comparative example I is 90.3%, and the retention rate after soaking of the comparative example II is 82.1%. The tensile strength of the prior industrially leading sabic GTX989 and Xuhua Xyron polyphenyl ether/nylon composite materials is greatly reduced by 88.6 percent and 86.9 percent respectively after the composite materials are soaked in ethylene glycol aqueous solution at high temperature.
Moisture absorption: ISO 62, 23 ℃. Example one is 1.5%.
Dielectric constant: IEC 62631,1MHz. Example one is 2.3.
Relative tracking index: IEC 60112. The first embodiment is 600V.
In the above ethylene glycol aqueous solution, the mass ratio of ethylene glycol to water was 50.
The raw materials of PA56/PA10T are all bio-based and meet the requirement of environmental protection; the PA56 and the PA10T endow the material with integral flexibility, PPO provides rigidity of the material and benzene rings exist, the PA10T can reduce decomposition of a PA56 molecular chain caused by ethylene glycol attack, the selection of the toughening agent improves the bonding performance of the PA/PPO, and in sum, alcoholysis resistance and electrical performance are improved. PA56 and PA10T are not flame-retardant, PPO and flame retardant are combined to endow flame retardant capability, the heat resistance of PA/PPO is improved in the presence of a toughening agent, and a nucleating agent is combined, so that on one hand, the formability is improved, on the other hand, the heat deformation is facilitated, and on the other hand, the VO flame retardant effect is achieved under the condition that the content of the flame retardant is less than 20% due to the stable and matched combination of main materials. In a word, the performance of the polyphenyl ether and nylon composite material is influenced by the selection of raw materials and the design of component content auxiliaries, in the invention, the dispersed phase particles of the alloy are refined and uniformly dispersed, and the resin winding structure is stable. The halogen-free flame-retardant alloy material can improve the combustibility of non-flame-retardant materials, achieves the UL94-V0 combustion grade, particularly can be made to be 0.4mm-V0, and particularly optimizes the combustibility of PA56/PA 10T; the alloy material has higher thermal performance (the thermal deformation can reach 150 ℃); the alloy material can improve the integral alcohol resistance, can pass a 135 ℃/1000H test and has the performance retention rate of over 90 percent; the alloy material reduces the moisture absorption rate of the conventional alloy material (most of PPO/PA), improves the dimensional stability, and particularly improves the moisture absorption of PA56 with higher moisture absorption; the alloy material has low dielectric constant and relative tracking index up to 600V.
Claims (10)
1. A halogen-free flame-retardant bio-based high-temperature-resistant nylon alloy/polyphenyl ether composite material is characterized by comprising PA56, PA10T, polyphenyl ether, a flame retardant, a toughening agent, a nucleating agent, an antioxidant and a lubricant.
2. The halogen-free flame-retardant bio-based high temperature resistant nylon alloy/polyphenylene oxide composite material according to claim 1, wherein the mass percentages of the PA56, the PA10T, the polyphenylene oxide, the flame retardant, the toughening agent, the nucleating agent, the antioxidant and the lubricant are respectively 10-20%, 20-50%, 10-30%, 10-20%, 5-10%, 1-3%, 0-1% and 0-1%.
3. The halogen-free flame-retardant bio-based high temperature resistant nylon alloy/polyphenylene oxide composite material according to claim 2, wherein the mass percentages of the PA56, the PA10T, the polyphenylene oxide, the flame retardant, the toughening agent, the nucleating agent, the antioxidant and the lubricant are respectively 10-20%, 30-40%, 15-25%, 15-20%, 5-10%, 1-3%, 0.3-0.8% and 0.3-0.7%.
4. The halogen-free flame-retardant bio-based high temperature resistant nylon alloy/polyphenylene oxide composite material as claimed in claim 1, wherein the flame retardant is one or more of organic hypophosphite, inorganic hypophosphite, melamine salt, polyphosphate and fluorine-containing anti-dripping agent.
5. The halogen-free flame-retardant bio-based high temperature resistant nylon alloy/polyphenylene oxide composite material according to claim 1, wherein the toughening agent is one or more of maleic anhydride grafted styrene-butadiene-styrene copolymer, maleic anhydride grafted hydrogenated styrene-butadiene-styrene copolymer, hydrogenated styrene-butadiene-styrene copolymer, and styrene-ethylene-propylene diblock polymer.
6. The halogen-free flame retardant bio-based high temperature resistant nylon alloy/polyphenylene oxide composite material as claimed in claim 1, wherein the nucleating agent is one or more of long chain saturated linear carboxylate, sorbitol compound, nonanol compound, xylitol compound, phosphorus compound and triaminobenzene derivative.
7. The halogen-free flame retardant bio-based high temperature resistant nylon alloy/polyphenylene oxide composite material as claimed in claim 1, wherein the antioxidant comprises copper salt antioxidant, hindered phenol antioxidant, hindered amine antioxidant, phosphite antioxidant, phosphate antioxidant, epoxy resin antioxidant; the lubricant is a silicon lubricant or an amide lubricant.
8. The preparation method of the halogen-free flame retardant bio-based high temperature resistant nylon alloy/polyphenylene oxide composite material according to claim 1, wherein the halogen-free flame retardant bio-based high temperature resistant nylon alloy/polyphenylene oxide composite material is obtained by melt mixing of PA56, PA10T, polyphenylene oxide, a flame retardant, a toughening agent, a nucleating agent, an antioxidant and a lubricant.
9. The use of the halogen-free flame retardant bio-based high temperature resistant nylon alloy/polyphenylene ether composite material of claim 1 in the preparation of flame retardant plastics.
10. The use of the halogen-free flame retardant bio-based high temperature resistant nylon alloy/polyphenylene ether composite material of claim 1 in the preparation of bio-based plastics.
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Cited By (5)
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| CN115873401A (en)* | 2022-12-27 | 2023-03-31 | 会通新材料股份有限公司 | Carbon fiber reinforced polyamide composition, preparation method and application |
| CN115926451A (en)* | 2022-12-10 | 2023-04-07 | 江苏沃特新材料科技有限公司 | Low-water-absorption nylon composite material and preparation method and application thereof |
| CN116875049A (en)* | 2023-08-04 | 2023-10-13 | 浙江科技学院 | A high-temperature nylon and polyphenylene ether alloy and its preparation method |
| CN117362979A (en)* | 2023-10-31 | 2024-01-09 | 创合新材料科技江苏有限公司 | Halogen-free flame-retardant PPO composite material and preparation method thereof |
| CN118085556A (en)* | 2022-11-28 | 2024-05-28 | 合肥杰事杰新材料股份有限公司 | High-performance creep-resistant low-expansion-coefficient PA66 composite material and preparation method thereof |
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