CN115637042A - Nitrogen-series flame-retardant nylon modified material with high glowing filament ignition temperature - Google Patents
Nitrogen-series flame-retardant nylon modified material with high glowing filament ignition temperature Download PDFInfo
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Abstract
The invention relates to a high glowing filament ignition temperature nitrogen-series flame-retardant nylon modified material which comprises the following components in parts by weight: 50-80 parts of modified nitrogen flame retardant MCA, 10-25 parts of modified alkali-free glass fiber and 0.5-5 parts of processing aid. According to the invention, the nitrogen flame retardant MCA and the zinc borate are subjected to composite modification, so that the particle diameter of the nitrogen flame retardant MCA is reduced, and the entanglement and crosslinking between the nitrogen flame retardant MCA and a nylon molecular chain are improved; meanwhile, the flame retardant synergy of the zinc borate further improves the flame retardant effect, reduces the usage amount and the cost, and reduces the mechanical property loss of the nylon. The silane modified alkali-free glass fiber is adopted, so that the interface binding force of the modified glass fiber on a nylon substrate is improved, the dispersibility is improved, and the strength and the toughness of the nylon material are improved. Different modified particles are blended with nylon, and a small amount of auxiliary agents such as a toughening agent and the like are added, so that the high glow-wire ignition temperature nitrogen-series flame-retardant nylon modified material with excellent mechanical property is obtained.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a high glowing filament ignition temperature nitrogen-series flame-retardant nylon modified material.
Background
Modern electronic and electrical equipment has more than 40% of parts by weight composed of flammable plastic insulating materials, and the electronic and electrical equipment can cause fire due to ignition of the materials caused by overheating, electric leakage, short circuit, spark, aging and the like, thereby causing great threat to the life and property safety of people. With the rapid development of the electronic and electrical appliance industry, the demand of industrial electrical appliances, household electrical appliances, automobile electrical appliances and the like for high-performance flame-retardant engineering plastics is increasing day by day. Such as high temperature resistant relays, high voltage electrical switches, transformer coil formers, delicate thin-walled electronic and electrical components, low voltage vacuum contactors, circuit breakers, and the like, require thermoplastic engineering plastics with high flame retardant properties, high toughness, and high Glow Wire Ignition Temperature (GWIT). The development of high-performance flame-retardant reinforced engineering plastics is one of the important directions for modifying the existing engineering plastics. A series of fire safety tests are carried out on the materials for the electronic and electrical equipment in Europe and America and other countries, and the results show that: the higher the flame retardancy of the materials used in the electronic and electrical equipment, the higher the fire safety of the equipment.
Among them, the flame retardant nylon (polyamide, PA) is widely used in important fields such as electronic and electric appliances due to its good flame retardancy and mechanical properties. PA is the most widely applied engineering plastic at present, the total output is the first of the world engineering plastics, and the glass fiber flame-retardant reinforced nylon composite material is widely applied to the fields of automobiles, mechanical instruments, electronics and electrics, national defense and military industry, aviation and the like. With the development of electronic and electrical equipment towards high performance and miniaturization, higher and higher requirements are also put forward on the performance of flame-retardant nylon.
The glass fiber nylon material has the characteristics of excellent mechanical strength, impact property, heat resistance, wear resistance, self-lubricating property, processability, mechanical balance and the like, and is widely applied to the industries of electronics, electrical and communication equipment, household electrical appliances, electromechanical equipment and the like. However, the glow wire temperature of the glass fiber flame-retardant reinforced polyamide composite material is difficult to reach 800 ℃, and the requirement of electronics and electrics on the high glow wire temperature of the material cannot be met. The domestic market of high-end polyamide engineering plastics is almost completely occupied by high-end products of a few international large companies, so that the development of the high glow-wire flame-retardant reinforced nylon material has great significance and wide development space.
In the prior art, fire protection is usually achieved by adding flame retardants. Research has shown that when a bromine-containing material is burned, brominated dibenzodioxin, polybrominated dibenzofuran, and the like are produced. It can decompose several highly toxic compounds at the halogen coordination sites, which damage the skin and liver, causing deformity and carcinogenesis. Other halogen flame retardant materials also emit toxic gases upon combustion and face the challenge of being strictly prohibited. Most of nylon materials are prepared by using a brominated flame retardant and antimony trioxide as flame retardants for synergistic use, and the material obtained by using the halogen-containing flame retardant has a good flame retardant effect, but once the material is combusted, a large amount of toxic gas and smoke are emitted, so that the physical and mental health of people is seriously harmed, and the requirement of people on safety cannot be met. While the inorganic non-halogen flame retardant can retard flame, the mechanical property of the material is adversely affected due to the large dosage. Therefore, people turn attention to another novel flame retardant, namely a nitrogen flame retardant. The nitrogen-based flame retardant for nylon mainly comprises modified melamine resin, melamine phosphate, melamine (MC), melamine Cyanurate (MCA) and the like, and the nitrogen-based flame retardant mainly comprises melamine and derivatives thereof and related heterocyclic compounds, and compounds with triazine structures. Most of the nitrogen flame retardants release NH by thermal decomposition 3 、N 2 、NO 2 And the like, generates the functions of heat absorption, temperature reduction, dilution and the like to achieve the purpose of flame retardance. Because the chemical properties of the flame retardant are very similar to those of nylon, the flame retardant has better application performance than halogen flame retardants and phosphorus flame retardants.
MCA has a very wide application as a flame retardant in nylon. The flame retarding mechanism of MCA includes three aspects, namely heat absorption, dilution and oxygen barrier. MCA can be decomposed into melamine and urate at high temperature, the melamine can be sublimated rapidly to absorb a large amount of heat, and the urate can catalyze and promote nylon to be decomposed into low molecular substances to form molten drops to transfer a large amount of heat to the environment. On the other hand, the generated gas can largely dilute the oxygen in the air, preventing the purpose of combustion. In addition, the blending of MCA and nylon does not blooming, does not adhere to a mold, has high thermal stability, and has very wide application as a flame retardant in nylon. However, as the MCA is less compatible with nylon resin, the tensile, flexural and impact strength of the material gradually decreases with increasing MCA addition.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a high glowing filament ignition temperature nitrogen-based flame-retardant nylon modified material.
The invention is realized by the following technical scheme:
a high glowing filament ignition temperature nitrogen-series flame-retardant nylon modified material comprises the following components in parts by weight:
50-80 parts of nylon resin, 10-25 parts of modified nitrogen flame retardant MCA, 15-25 parts of modified alkali-free glass fiber and 0.5-5 parts of processing aid.
Further, the nitrogen-based flame retardant MCA was modified by the following method: mixing zinc borate and MCA according to the mass ratio of 1.
And the zinc borate microcrystals separated out after modification are dispersed and deposited on the surface of MCA to induce the formation of MCA micromolecules. The molecular structure of MCA modified by zinc borate is not changed, and the modified MCA has small particle size and regular appearance, and is beneficial to dispersion in nylon materials. In addition, zinc borate is one of the most important boron flame retardants, and is mainly characterized in that: (1) The flame retardant has synergistic effect and synergistic effect, and can effectively reduce the smoke amount in the combustion of the material. (2) Promoting the generation of a carbon layer, and the carbon layer can be B 2 O 3 And (4) stabilizing. (3) Prevent the generation of molten drops due toThereby reducing the harmfulness of the secondary fire caused by the molten drops.
Further, the alkali-free glass fiber is modified by the following method: the surface of the alkali-free glass fiber is pretreated by adopting a silane coupling agent, and the adding amount of the silane coupling agent is 0.1-2 wt% of the alkali-free glass fiber. The silane coupling agent is 3- (methacryloyloxy) propyl trimethoxy silane.
A certain amount of silane coupling agent 3- (methacryloyloxy) propyl trimethoxy silane (KH 570) is added to modify the alkali-free chopped glass fiber, so that the compatibility of the glass fiber and a nylon matrix is improved, and the mechanical property of the nylon is further enhanced.
Further, the processing aid comprises a compatibilizer which is ethylene-butyl acrylate, a toughening agent which is ethylene-methyl acrylate-glycidyl methacrylate terpolymer, an antioxidant which is bis (octadecyl) pentaerythritol diphosphite, and the compatibilizer is: a toughening agent: the mass ratio of the antioxidant is 2.
The preparation method of the high glowing filament ignition temperature nitrogen-series flame-retardant nylon modified material adopts the following steps: and (2) fully mixing the modified nitrogen flame retardant MCA, the nylon and the processing aid in a high-speed mixer, adding the mixture into a double-screw extruder, adding the modified alkali-free glass fiber through a glass fiber port of the screw extruder, carrying out melt extrusion at the extrusion temperature of 190-250 ℃ and the screw rotation speed of 300-400r/min, and finally cooling, air-drying and dicing the extruded material to obtain the high glow wire ignition temperature nitrogen flame-retardant nylon modified material.
The invention has the following beneficial effects:
1) The composite modification of the nitrogen flame retardant MCA is realized by a new method. Through co-dissolving with zinc borate and then recrystallizing. The precipitated zinc borate microcrystals are dispersed and deposited on the surface of MCA to induce the formation of MCA micromolecules. The MCA molecular structure modified by the zinc borate is not changed, and the modified MCA particles have small particle size and regular appearance, thereby being beneficial to the dispersion in the nylon material matrix. In addition, a small amount of zinc borate is added to play a role in flame retardance and synergy;
2) Realizes the surface modification of the alkali-free glass fiber, improves the interface and the structure of the glass fiber and a nylon matrix, and enhances the mechanical property of the glass fiber and the nylon matrix. The silane coupling agent 3- (methacryloyloxy) propyl trimethoxy silane (KH 570) further modifies the glass fiber, and improves the compatibility and the dispersibility of the alkali-free glass fiber and a nylon matrix, thereby obtaining the high-performance composite nylon material.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a schematic diagram of the preparation of composite modified MCA;
FIG. 3 is a schematic view of a modified alkali-free glass fiber reinforced nylon matrix.
Detailed Description
The invention is described in further detail below with reference to the accompanying drawings in order to better understand the technical solution.
Complex modification of MCA
MCA is a molecular complex formed by compounding Melamine (ME) and Cyanuric Acid (CA), and the two can form nine hydrogen bonds in three-dimensional direction to form a huge hydrogen bond grid with a regular structure. MCA is a novel high-efficiency polyamide flame retardant. However, as the amount of MCA added increases, the tensile, flexural and impact strength of the material gradually decreases due to the poor compatibility of MCA with nylon.
In the experiment, MCA and zinc borate are mixed and dissolved to be separated out, and the separated zinc borate microcrystals are dispersed and deposited on the surface of MCA to induce the formation of MCA micromolecules. The molecular structure of MCA modified by zinc borate is not changed, and the modified MCA has small particle size and regular appearance, and is beneficial to dispersion in nylon materials. A schematic of the preparation of MCA modification is shown in FIG. 2.
Improvement of flame retardancy
The glass fiber plays a role of a wick in the combustion process of nylon to promote combustion, but the mechanism research on the wick effect of the glass fiber is not sufficient at present, but the wick effect is generally considered to be related to the interface property between a polymer melt phase and the glass fiber and the infiltration process of the melt phase on the surface of the glass fiber, and the infiltration driving force is directly influenced by the viscosity of the melt. Because the traditional MCA flame-retardant nylon mainly has the mechanism of sublimation heat absorption and decomposition products for catalyzing nylon to be decomposed into oligomers to promote molten drop formation and transfer heat, and the condensed phase process is relatively weak, the melt phase viscosity of the traditional MCA flame-retardant system is greatly reduced in the combustion process, so that the infiltration driving force is increased, the candle wick effect is enhanced, and the traditional MCA has poor flame-retardant effect on glass fiber reinforced nylon materials.
This experiment solved this problem by adding zinc borate. The zinc borate modified MCA not only improves the dispersibility of the modified MCA particles, but also reduces the dosage of the MCA by utilizing the flame retardant synergy of the zinc borate. Zinc borate is one of the most important boron-based flame retardants, and is mainly used as an inorganic flame retardant additive. The main characteristics are as follows: (1) The flame retardant has synergistic effect and synergistic effect, and can effectively reduce the smoke quantity in the combustion of the material. (2) Promoting the generation of carbon layer, and the carbon layer can be B2O3 stable. (3) The formation of molten droplets is prevented, and the hazard of secondary fire caused by molten droplets is reduced. A schematic diagram of the modified alkali-free glass fiber reinforced nylon matrix is shown in fig. 3.
Because the structures and properties of Glass Fiber (GF) and nylon are greatly different, in order to improve the structures and properties of GF and nylon interfaces and improve the mechanical property of the composite material, silane coupling agent KH570 is selected to pretreat the surface of the glass fiber. The coupling agent effectively improves the bonding property of the GF and the nylon interface, so that the GF can effectively play a role in transferring load and dissipating energy, and the impact strength and the tensile strength of the glass fiber reinforced nylon material treated by the coupling agent are higher than those of the glass fiber reinforced nylon material without the coupling agent.
The technical route of the invention is shown in figure 1, the nitrogen flame retardant MCA and the zinc borate are subjected to composite modification, the particle diameter of the nitrogen flame retardant MCA is reduced, the entanglement and crosslinking between the nitrogen flame retardant MCA and a nylon molecular chain are improved, and the dispersibility is improved. Meanwhile, the flame retardant synergy of the zinc borate further improves the flame retardant effect, reduces the usage amount and the cost, and reduces the mechanical property loss of the nylon. The modified alkali-free glass fiber is prepared by adopting a silane modification process, the interface binding force of the modified glass fiber on a nylon matrix is improved, the dispersibility is improved, the stability is higher, and the strength and the toughness of the nylon material are improved. Different modified particles are blended with nylon, a small amount of auxiliary agents such as a toughening agent and the like are added, and the processing technology is improved, so that the high glowing filament ignition temperature nitrogen-series flame-retardant nylon modified material with excellent mechanical property is obtained. The composite modified MCA flame-retardant glass fiber reinforced nylon modified material is a new high-performance flame-retardant material, and research, development and industrial application of the material provide a new technical approach for expanding the matching and industrial application of plastic processing materials, so that the sustainable development and application of nylon in the electronic industry are realized, and the plastic processing industry is really improved for the people-friendly industry of life health and safety of people.
Example 1
Co-dissolving a small amount of zinc borate and MCA until crystals are precipitated and dried, wherein the solid content ratio of the zinc borate to the MCA is 1:1000. 0.1wt% of silane coupling agent KH570 is added to modify the alkali-free chopped glass fiber, improve the compatibility of the glass fiber and the nylon matrix and further enhance the mechanical property of the nylon. 50 parts of nylon, 20 parts of flame retardant modified MCA and 5 parts of auxiliary agents such as a compatibilizer, a flexibilizer, an antioxidant and the like are placed in a high-speed stirrer to be fully mixed, then a double-screw extruder is added, 25 parts of modified GF is added through a GF port of the screw extruder, and the flame-retardant reinforced nylon granules are obtained through extrusion, cooling and grain cutting.
Example 2
Co-dissolving a small amount of zinc borate and MCA until crystals are precipitated and dried, wherein the solid content ratio of the zinc borate to the MCA is 1:500. 0.5wt% of silane coupling agent KH570 is added to modify the alkali-free chopped glass fiber, improve the compatibility of the glass fiber and the nylon matrix and further enhance the mechanical property of the nylon. And (2) putting 65 parts of nylon, 20 parts of flame retardant modified MCA and 5 parts of auxiliary agents such as a compatibilizer, a toughening agent, an antioxidant and the like into a high-speed stirrer for full mixing, then adding the mixture into a double-screw extruder, adding 15 parts of modified GF through a GF port of the screw extruder, extruding, cooling and granulating to obtain the flame-retardant reinforced nylon granules.
Example 3
Co-dissolving a small amount of zinc borate and MCA until crystals are precipitated and dried, wherein the solid content ratio of the zinc borate to the MCA is 1:100. 2wt% of silane coupling agent KH570 is added to modify the alkali-free chopped glass fiber, improve the compatibility of the glass fiber and the nylon matrix, and further enhance the mechanical properties of the nylon. And (2) putting 80 parts of nylon, 10 parts of flame retardant modified MCA and 0.5 part of auxiliary agents such as a compatibilizer, a flexibilizer, an antioxidant and the like into a high-speed stirrer for full mixing, then adding into a double-screw extruder, adding 20 parts of modified GF through a GF port of the screw extruder, extruding, cooling and granulating to obtain the flame-retardant reinforced nylon granules.
Example 4
And (2) co-dissolving a small amount of zinc borate and MCA until crystals are precipitated and dried, wherein the solid content ratio of the zinc borate to the MCA is 1:20. 1.5wt% of silane coupling agent KH570 is added to modify the alkali-free chopped glass fiber, improve the compatibility of the glass fiber and the nylon matrix, and further enhance the mechanical property of the nylon. And (3) putting 70 parts of nylon, 12 parts of flame retardant modified MCA and 3 parts of auxiliary agents such as a compatibilizer, a toughening agent, an antioxidant and the like into a high-speed stirrer for full mixing, then adding into a double-screw extruder, adding 15 parts of modified GF through a GF port of the double-screw extruder, extruding, cooling and granulating to obtain the flame-retardant reinforced nylon granules.
Comparative example 1
And (2) putting 75 parts of nylon, 10 parts of flame retardant modified MCA and 1 part of auxiliary agents such as a compatibilizer, a toughening agent, an antioxidant and the like into a high-speed stirrer for full mixing, then adding the mixture into a double-screw extruder, adding 14 parts of modified GF through a GF port of the screw extruder, extruding, cooling and granulating to obtain the flame-retardant reinforced nylon granules.
The properties of the nylon pellets obtained in the above examples and comparative examples are compared in Table 1.
TABLE 1
As can be seen from Table 1, after the zinc borate modified MCA is added in a certain proportion, the flame retardance of the nylon composite material is obviously improved; when the tensile strength and the bending strength are improved along with the increase of KH570 in the alkali-free glass fiber, the mechanical property of the composite film is gradually improved. This indicates an improvement in the performance of the flame retardant nylon by the modified MCA.
Claims (6)
1. A high glowing filament ignition temperature nitrogen-based flame-retardant nylon modified material is characterized by comprising the following components in parts by weight:
50-80 parts of nylon resin, 10-25 parts of modified nitrogen flame retardant MCA, 15-25 parts of modified alkali-free glass fiber and 0.5-5 parts of processing aid.
2. The modified nitrogen-based flame-retardant nylon material with high glowing filament ignition temperature of claim 1, wherein the nitrogen-based flame retardant MCA is modified by the following method:
mixing zinc borate and MCA according to the mass ratio of 1.
3. The modified nitrogen-based flame-retardant nylon material with high glowing filament ignition temperature of claim 1, wherein the alkali-free glass fiber is modified by the following method:
the surface of the alkali-free glass fiber is pretreated by adopting a silane coupling agent, and the adding amount of the silane coupling agent is 0.1-2 wt% of the alkali-free glass fiber.
4. The modified nylon material with high glowing filament ignition temperature of claim 3, wherein the silane coupling agent is 3- (methacryloyloxy) propyl trimethoxy silane.
5. The modified nitrogen-based flame retardant nylon material with high glowing filament ignition temperature of claim 1, wherein the processing aid comprises a compatibilizer ethylene-butyl acrylate, a toughener ethylene-methyl acrylate-glycidyl methacrylate terpolymer and an antioxidant bis (octadecyl) pentaerythritol diphosphite, wherein the compatibilizer: a toughening agent: the mass ratio of the antioxidant is 2.
6. The preparation method of the high glowing filament ignition temperature nitrogen-series flame-retardant nylon modified material of any one of claims 1 to 5 is characterized by comprising the following steps:
and (2) fully mixing the modified nitrogen flame retardant MCA, the nylon and the processing aid in a high-speed mixer, adding the mixture into a double-screw extruder, adding the modified alkali-free glass fiber through a glass fiber port of the screw extruder, carrying out melt extrusion at the extrusion temperature of 190-250 ℃ and the screw rotation speed of 300-400r/min, and finally cooling, air-drying and dicing the extruded material to obtain the high glow wire ignition temperature nitrogen flame-retardant nylon modified material.
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