CN118185273A - A high-strength flame-retardant PC material and its production process - Google Patents
A high-strength flame-retardant PC material and its production process Download PDFInfo
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Abstract
The invention relates to the technical field of plastic engineering, in particular to a high-strength flame-retardant PC material and a production process thereof; the high-strength flame-retardant PC material comprises the following raw materials in parts by weight: 80 to 100 parts of PC resin, 35 to 45 parts of ABS resin, 20 to 30 parts of glass fiber, 1.0 to 1.8 parts of 3-aminopropyl triethoxysilane, 2 to 3 parts of 3-potassium benzenesulfonyl benzenesulfonate, 3 to 6 parts of nano titanium dioxide, 2 to 4 parts of pentaerythritol stearate, 3 to 5 parts of compatilizer, 5 to 8 parts of toughener, 4 to 6 parts of composite flame retardant, 1.5 to 2.5 parts of antioxidant and 15 to 20 parts of inorganic filler; the PC material produced by the invention not only has better mechanical property, but also has excellent ageing resistance and flame retardant property, effectively prolongs the service life and ensures the quality.
Description
Technical Field
The invention relates to the technical field of plastic engineering, in particular to a high-strength flame-retardant PC material and a production process thereof.
Background
Polycarbonate, PC for short, is a widely used material with excellent comprehensive properties, and is common in life, such as beverage bottles, plastic bags and the like; the rubber has high height, elastic coefficient, high impact strength and wide use temperature range; high transparency and free dyeing properties; the molding shrinkage is low, and the dimensional stability is good; the product is odorless and harmless to human body, and meets the sanitary and safe advantages. Because of the advantages, the novel high-performance composite material is widely applied to the fields of construction, automobiles, medicines, capital construction, ships, aerospace and the like.
A high-strength wear-resistant PC material and a preparation process thereof are disclosed in a patent document with the application number of CN 202210948250.2; firstly, microcrystalline cellulose is used as a raw material to prepare nano-scale nano microcrystalline cellulose, under the activation of 1-ethyl- (3-dimethylaminopropyl) carbodiimide, hydroxyl groups on the surface of the nano microcrystalline cellulose are replaced by epoxy groups, the epoxy groups react with high-pressure CO 2 gas under a catalytic condition to realize the ring opening of the epoxy groups, the modified nano cellulose with carbonate monomers is obtained, and then a diol compound is used to generate polycarbonate, so that the modified nano cellulose can be effectively dispersed in a polycarbonate matrix, the binding capacity of the modified nano cellulose is enhanced, the stress applied to the surface of the polycarbonate can be dispersed, and damage caused by stress concentration is avoided, thereby effectively enhancing the wear resistance and strength of the polycarbonate.
The PC material prepared by the patent document has better wear resistance and mechanical strength, but relatively poorer ageing resistance, and shortens the service life to a certain extent. Moreover, the flame retardant performance is relatively insufficient, and when a fire disaster happens accidentally in the use process, the loss and the harm caused by the fire disaster cannot be avoided. Therefore, the invention provides a high-strength flame-retardant PC material and a production process thereof, which are used for solving the technical problems.
Disclosure of Invention
The invention aims to provide a high-strength flame-retardant PC material and a production process thereof, and the produced PC material not only has better mechanical properties, but also has excellent ageing resistance and flame retardance, thereby effectively prolonging the service life and guaranteeing the quality.
In order to achieve the above purpose, the present invention provides the following technical solutions:
A high-strength flame-retardant PC material consists of the following raw materials in parts by weight: 80 to 100 parts of PC resin, 35 to 45 parts of ABS resin, 20 to 30 parts of glass fiber, 1.0 to 1.8 parts of 3-aminopropyl triethoxysilane, 2 to 3 parts of 3-potassium benzenesulfonyl benzenesulfonate, 3 to 6 parts of nano titanium dioxide, 2 to 4 parts of pentaerythritol stearate, 3 to 5 parts of compatilizer, 5 to 8 parts of toughener, 4 to 6 parts of composite flame retardant, 1.5 to 2.5 parts of antioxidant and 15 to 20 parts of inorganic filler;
the composite flame retardant takes an inorganic substrate as a core, takes a modifier as a first shell, takes a product generated by the chemical reaction of a reaction intermediate and 2, 6-di-tert-butyl-4-methylphenol as a second shell, and has an obvious core-shell structure; the inorganic substrate is porous nano magnesium hydroxide with a ball-like flower-like structure;
Wherein, the PC resin is bisphenol A type polycarbonate with the molecular weight of 20000-30000;
the ABS resin is a copolymer of acrylonitrile, butadiene and styrene, wherein the percentage content of butadiene is 20-30%;
The glass fiber is alkali-free chopped glass fiber, the diameter of the glass fiber is 5-10 mu m, and the chopping length is 3-5 mm.
Furthermore, the compatilizer is selected from any one of PP-g-MA and PS-g-PMMA.
Further, the antioxidant is any one of antioxidant 1010, antioxidant 1076 and antioxidant 168.
Further, the inorganic filler is any one of aluminum nitride, aluminum oxide and silicon carbide; and the particle size is 5-15 mu m.
Furthermore, the toughening agent is any one of EMA, MBS, POE and high-glue powder.
Further, the preparation method of the composite flame retardant comprises the following steps:
Step one, tetraphosphoric acid and ethylene oxide are mixed according to the proportion of 1: mixing and stirring evenly in a mass ratio of 2-5, and reacting for 2-3 h under the conditions that the pressure is lower than 0.15MPa and the temperature is 50-60 ℃ after the replacement of inert gas; after the reaction is finished, aminobenzene with the mass 1-2 times of that of ethylene oxide is added into the obtained product components, and the mixture is subjected to heat preservation reaction for 100-150 min at the temperature of 60-80 ℃ under the pressure of lower than 0.15 MPa; after the reaction is finished, the obtained product is a reaction intermediate;
Sequentially adding the modified inorganic substrate and the 2, 6-di-tert-butyl-4-methylphenol into ethanol according to the dosage ratio of 0.002-0.004 g/mL and 0.003-0.005 g/mL, uniformly mixing and stirring, placing the obtained mixture into an oil bath pot, heating to 60-70 ℃ under magnetic stirring, adding ethanol dispersion liquid of a reaction intermediate with the volume of 3-5 times and the concentration of 0.005-0.008 g/mL into the obtained mixture phase, uniformly dispersing, and then carrying out heat preservation reaction for 30-40 h under the protection of nitrogen; and after the reaction is finished, evaporating ethanol in the components of the obtained product, and vacuum drying the obtained solid product to constant weight at the temperature of 80-90 ℃ to obtain the composite flame retardant.
Further, the preparation method of the modified inorganic substrate comprises the following steps:
Uniformly dispersing the o-hydroxybenzoic acid into thionyl chloride according to the solid-to-liquid ratio of 0.02-0.03 g/mL, and stopping the reaction when the reflux reaction is carried out until no irritant gas escapes; then evaporating out the residual thionyl chloride in the reaction system to obtain the modifier;
II, ultrasonically dispersing the pretreated inorganic substrate in chloroform according to the solid-liquid ratio of 0.01-0.02 g/mL, and sequentially adding 40-60% of modifier and 3-5% of triethylamine by mass of the pretreated inorganic substrate; after being uniformly mixed, nitrogen is introduced, and stirring reaction is carried out until no irritant gas escapes; and filtering the obtained product components, alternately washing the obtained filter cake with chloroform and ethanol for 2-3 times, and performing vacuum drying treatment to obtain the modified inorganic substrate.
Further, the preparation method of the pretreated inorganic substrate comprises the following steps: uniformly dispersing an inorganic substrate in N, N-dimethylformamide according to a solid-to-liquid ratio of 0.005-0.01 g/mL, then adding 3-aminopropyl trimethoxysilane with the mass of 20-30% of the inorganic substrate into the N, N-dimethylformamide, uniformly mixing and stirring, and carrying out reflux reaction for 8-12 h; and after the reaction is finished, carrying out solid-liquid separation on the obtained product components, and sequentially carrying out water washing and vacuum drying treatment on the obtained filter cake to obtain the pretreated inorganic substrate.
Further, the preparation method of the inorganic substrate comprises the following steps: adding 20-35% glycol into 1-2 mol/L magnesium nitrate aqueous solution, mixing and stirring uniformly, then slowly dripping 2-4 mol/L potassium hydroxide aqueous solution into the obtained mixed solution, stirring at a speed of 1000-2000 r/min for reaction for 20-30 h, aging the obtained precipitate for 3-6 h after the reaction is finished, filtering, washing the obtained filter cake with deionized water until no nitrate ions are detected, washing with absolute ethyl alcohol for 2-3 times, and vacuum drying the washed solid powder to constant weight at a temperature of 70-100 ℃ to obtain the inorganic substrate.
A production process of a high-strength flame-retardant PC material comprises the following steps: accurately weighing all raw materials required for producing the high-strength flame-retardant PC material, and then drying the raw materials at the temperature of 80-100 ℃ for 8-12 hours respectively; after the drying is finished, mixing and stirring the raw materials uniformly at the temperature of 50-65 ℃, transferring the obtained mixed materials into a double-screw extruder for blending, and carrying out melt extrusion granulation to obtain the high-strength flame-retardant PC material;
Wherein, each district temperature of twin-screw machine is respectively: the rotation speed of the machine head is set to 320-450 r/min at 225 ℃ in the first region, 230 ℃ in the second region, 245 ℃ in the third region, 260 ℃ in the fourth region, 270 ℃ in the fifth region, 255 ℃ in the sixth region, 265 ℃ in the seventh region, 270 ℃ in the eighth region, 275 ℃ in the ninth region and 280 ℃ in the first region.
Compared with the prior art, the invention has the beneficial effects that:
In the invention, magnesium nitrate, glycol, potassium hydroxide and the like are used as raw materials, and a hydrothermal method is adopted to prepare the porous nano magnesium hydroxide-inorganic base material with a ball-like flower-like structure. Then 3-aminopropyl trimethoxy silane is used for pretreatment of the inorganic substrate, the obtained pretreated inorganic substrate is dispersed in chloroform in an ultrasonic way, then chemical reaction is carried out on the pretreated inorganic substrate and a modifier under the action of triethylamine, and finally the modifier is grafted on the surface of the pretreated inorganic substrate under the action of triethylamine. The ultraviolet aging resistance of the inorganic substrate is obviously improved due to the grafting of the modifier.
The obtained modified inorganic base material and 2, 6-di-tert-butyl-4-methylphenol are sequentially put into ethanol, the reaction intermediate is added after being mixed and stirred uniformly, the 2, 6-di-tert-butyl-4-methylphenol which is retained in the pore structure of the inorganic base material and the reaction intermediate are subjected to thermal insulation reaction, hydroxyl in the 2, 6-di-tert-butyl-4-methylphenol and the reaction intermediate are subjected to chemical reaction to form bonds in the reaction process, the nitrogen-and phosphorus-containing products obtained by the reaction of the two products have good flame retardance, and the dense staggered coating of the nitrogen-and phosphorus-containing products forms an enveloping structure of a three-dimensional network on the surface of the modified inorganic base material, so that the composite flame retardant finished product is finally prepared. The obtained composite flame retardant takes an inorganic substrate as a core, takes a modifier as a first shell, takes a product generated by the chemical reaction of a reaction intermediate and 2, 6-di-tert-butyl-4-methylphenol as a second shell, and has an obvious core-shell structure. Finally, the flame retardant property of the prepared PC material is obviously improved under the synergistic combination of the inorganic base material and the generated chemical product. Meanwhile, the modifier and the 2, 6-di-tert-butyl-4-methylphenol are mutually synergistic, so that the ageing resistance of the PC material is effectively improved. And the mechanical properties of the PC material are also effectively ensured by using the glass fiber and the toughening agent.
In conclusion, the PC material produced by the invention has better mechanical property, excellent ageing resistance and flame retardant property, effectively prolongs the service life and ensures the quality.
Drawings
FIG. 1 is an infrared spectrum of the reaction intermediate prepared in example 1.
FIG. 2 is an infrared spectrum of the modifier prepared in example 1.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A high-strength flame-retardant PC material consists of the following raw materials in parts by weight: 80 parts of PC resin, 35 parts of ABS resin, 20 parts of glass fiber, 1.0 part of 3-aminopropyl triethoxysilane, 2 parts of 3-benzenesulfonyl potassium benzenesulfonate, 3 parts of nano titanium dioxide, 2 parts of pentaerythritol stearate, 3 parts of compatilizer PP-g-MA, 5 parts of toughening agent EMA, 4 parts of composite flame retardant, 1.5 parts of antioxidant 1010 and 15 parts of aluminum nitride with the grain diameter of 5 mu m;
the composite flame retardant takes an inorganic substrate as a core, takes a modifier as a first shell, takes a product generated by the chemical reaction of a reaction intermediate and 2, 6-di-tert-butyl-4-methylphenol as a second shell, and has an obvious core-shell structure; the inorganic substrate is porous nano magnesium hydroxide with a ball-like flower-like structure;
Wherein, the PC resin is bisphenol A polycarbonate with the molecular weight of 20000;
The ABS resin is a copolymer of acrylonitrile, butadiene and styrene, wherein the percentage content of butadiene is 20%;
The glass fiber was alkali-free chopped glass fiber having a diameter of 5 μm and a chopped length of 3mm.
The preparation method of the composite flame retardant comprises the following steps:
Step one, tetraphosphoric acid and ethylene oxide are mixed according to the proportion of 1:2, uniformly mixing and stirring, and reacting for 2 hours under the conditions that the pressure is lower than 0.15MPa and the temperature is 50 ℃ after the replacement of inert gas; after the reaction is finished, aminobenzene with the mass equal to that of ethylene oxide is added into the obtained product components, and the mixture is subjected to heat preservation reaction for 100min at the temperature of 60 ℃ and the pressure of which is lower than 0.15 MPa; after the reaction is finished, the obtained product is a reaction intermediate;
Sequentially adding the modified inorganic substrate and the 2, 6-di-tert-butyl-4-methylphenol into ethanol according to the dosage ratio of 0.002g/mL and 0.003g/mL, uniformly mixing and stirring, placing the obtained mixture into an oil bath pot, heating to 60 ℃ under magnetic stirring, adding an ethanol dispersion liquid of a reaction intermediate with the volume of 3 times and the concentration of 0.005g/mL into the obtained mixed phase, uniformly dispersing, and then carrying out heat preservation reaction for 30 hours under the protection of nitrogen; and after the reaction is finished, evaporating ethanol in the components of the obtained product, and vacuum drying the obtained solid product at the temperature of 80 ℃ to constant weight to obtain the composite flame retardant.
The preparation method of the modified inorganic substrate comprises the following steps:
Uniformly dispersing the o-hydroxybenzoic acid in thionyl chloride according to the solid-to-liquid ratio of 0.02g/mL, and stopping the reaction when the reflux reaction is carried out until no irritant gas escapes; then evaporating out the residual thionyl chloride in the reaction system to obtain the modifier;
II, ultrasonically dispersing the pretreated inorganic substrate in chloroform according to a solid-to-liquid ratio of 0.01g/mL, and sequentially adding a modifier with the mass of 40% of the pretreated inorganic substrate and 3% of triethylamine; after being uniformly mixed, nitrogen is introduced, and stirring reaction is carried out until no irritant gas escapes; and filtering the obtained product components, alternately washing the obtained filter cake with chloroform and ethanol for 2 times, and performing vacuum drying treatment to obtain the modified inorganic substrate.
The preparation method of the pretreated inorganic substrate comprises the following steps: uniformly dispersing an inorganic substrate in N, N-dimethylformamide according to a solid-to-liquid ratio of 0.005g/mL, then adding 3-aminopropyl trimethoxysilane with the mass being 20% of that of the inorganic substrate into the N, N-dimethylformamide, uniformly mixing and stirring, and then carrying out reflux reaction for 8 hours; and after the reaction is finished, carrying out solid-liquid separation on the obtained product components, and sequentially carrying out water washing and vacuum drying treatment on the obtained filter cake to obtain the pretreated inorganic substrate.
The preparation method of the inorganic substrate comprises the following steps: adding 20% glycol into 1mol/L magnesium nitrate aqueous solution, mixing and stirring uniformly, slowly dripping 2mol/L potassium hydroxide aqueous solution with the same volume as the magnesium nitrate aqueous solution into the obtained mixed solution, stirring and reacting for 20 hours at the speed of 1000r/min, aging the obtained precipitate for 3 hours after the reaction is finished, filtering, washing the obtained filter cake with deionized water until no nitrate ions are detected, washing with absolute ethyl alcohol for 2 times, and vacuum drying the solid powder obtained after washing at the temperature of 70 ℃ until the weight is constant, thus obtaining the inorganic substrate.
A production process of a high-strength flame-retardant PC material comprises the following steps: accurately weighing all raw materials required for producing the high-strength flame-retardant PC material, and then drying the raw materials at the temperature of 80 ℃ for 8 hours respectively; after the drying is finished, mixing and stirring the raw materials uniformly at 50 ℃, transferring the obtained mixture into a double-screw extruder for blending, and carrying out melt extrusion granulation to obtain the high-strength flame-retardant PC material;
Wherein, each district temperature of twin-screw machine is respectively: the rotation speed of the machine head is set to 320r/min, namely 225 ℃ in the first area, 230 ℃ in the second area, 245 ℃ in the third area, 260 ℃ in the fourth area, 270 ℃ in the fifth area, 255 ℃ in the sixth area, 265 ℃ in the seventh area, 270 ℃ in the eighth area, 275 ℃ in the ninth area and 280 ℃ in the machine head.
Example 2
The production process of the high-strength flame-retardant PC material in this embodiment is basically the same as that of embodiment 1, except that: the specific proportion of the raw materials used by the high-strength flame-retardant PC material and the preparation method of the composite flame retardant are different; the specific proportion of the raw materials used for the high-strength flame-retardant PC material and the preparation method of the composite flame retardant in the embodiment are as follows:
A high-strength flame-retardant PC material consists of the following raw materials in parts by weight: 90 parts of PC resin, 40 parts of ABS resin, 25 parts of glass fiber, 1.5 parts of 3-aminopropyl triethoxysilane, 2.5 parts of 3-benzenesulfonyl potassium benzenesulfonate, 5 parts of nano titanium dioxide, 3 parts of pentaerythritol stearate, 4 parts of compatilizer PS-g-PMMA, 6 parts of toughening agent MBS, 5 parts of composite flame retardant, 2 parts of antioxidant 1076 and 16 parts of alumina with the particle size of 10 mu m.
The preparation method of the composite flame retardant comprises the following steps:
Step one, tetraphosphoric acid and ethylene oxide are mixed according to the proportion of 1:3, uniformly mixing and stirring, and reacting for 2.5 hours under the conditions that the pressure is lower than 0.15MPa and the temperature is 55 ℃ after the replacement of inert gas; after the reaction is finished, aminobenzene with the mass 1.5 times of that of ethylene oxide is added into the obtained product components, and the mixture is subjected to heat preservation reaction for 120min at the temperature of 70 ℃ and the pressure of which is lower than 0.15 MPa; after the reaction is finished, the obtained product is a reaction intermediate;
Sequentially adding the modified inorganic substrate and the 2, 6-di-tert-butyl-4-methylphenol into ethanol according to the dosage ratio of 0.003g/mL and 0.004g/mL, uniformly mixing and stirring, placing the obtained mixture into an oil bath pot, heating to 65 ℃ under magnetic stirring, adding an ethanol dispersion liquid of a reaction intermediate with the volume of 4 times and the concentration of 0.006g/mL into the obtained mixed phase, uniformly dispersing, and then carrying out heat preservation reaction for 35h under the protection of nitrogen; and after the reaction is finished, evaporating ethanol in the components of the obtained product, and vacuum drying the obtained solid product at the temperature of 85 ℃ to constant weight to obtain the composite flame retardant.
The preparation method of the modified inorganic substrate comprises the following steps:
Uniformly dispersing the o-hydroxybenzoic acid in thionyl chloride according to the solid-to-liquid ratio of 0.025g/mL, and stopping the reaction when the reflux reaction is carried out until no irritant gas escapes; then evaporating out the residual thionyl chloride in the reaction system to obtain the modifier;
II, ultrasonically dispersing the pretreated inorganic substrate in chloroform according to a solid-to-liquid ratio of 0.015g/mL, and sequentially adding a modifier with the mass of 50% of the pretreated inorganic substrate and triethylamine with the mass of 4%; after being uniformly mixed, nitrogen is introduced, and stirring reaction is carried out until no irritant gas escapes; and filtering the obtained product components, alternately washing the obtained filter cake with chloroform and ethanol for 2 times, and performing vacuum drying treatment to obtain the modified inorganic substrate.
The preparation method of the pretreated inorganic substrate comprises the following steps: uniformly dispersing an inorganic substrate in N, N-dimethylformamide according to a solid-liquid ratio of 0.008g/mL, then adding 3-aminopropyl trimethoxy silane with the mass being 25% of that of the inorganic substrate into the N, N-dimethylformamide, uniformly mixing and stirring, and then carrying out reflux reaction for 10h; and after the reaction is finished, carrying out solid-liquid separation on the obtained product components, and sequentially carrying out water washing and vacuum drying treatment on the obtained filter cake to obtain the pretreated inorganic substrate.
The preparation method of the inorganic substrate comprises the following steps: adding 30% glycol into 1.5mol/L magnesium nitrate aqueous solution, mixing and stirring uniformly, slowly dripping 3mol/L potassium hydroxide aqueous solution with the same volume as the magnesium nitrate aqueous solution into the obtained mixed solution, stirring and reacting for 25 hours at a speed of 1500r/min, aging the obtained precipitate for 5 hours after the reaction is finished, filtering, washing the obtained filter cake with deionized water until no nitrate ions are detected, washing with absolute ethyl alcohol for 2 times, and vacuum drying the solid powder obtained after washing at 80 ℃ until the weight is constant, thus obtaining the inorganic substrate.
Example 3
The production process of the high-strength flame-retardant PC material in this embodiment is basically the same as that of embodiment 1, except that: the specific proportion of the raw materials used by the high-strength flame-retardant PC material and the preparation method of the composite flame retardant are different; the specific proportion of the raw materials used for the high-strength flame-retardant PC material and the preparation method of the composite flame retardant in the embodiment are as follows:
A high-strength flame-retardant PC material consists of the following raw materials in parts by weight: 100 parts of PC resin, 45 parts of ABS resin, 30 parts of glass fiber, 1.8 parts of 3-aminopropyl triethoxysilane, 3 parts of 3-benzenesulfonyl potassium benzenesulfonate, 6 parts of nano titanium dioxide, 4 parts of pentaerythritol stearate, 5 parts of compatilizer PP-g-MA, 8 parts of toughening agent POE, 6 parts of composite flame retardant, 2.5 parts of antioxidant 168 and 20 parts of silicon carbide with the particle size of 15 mu m.
The preparation method of the composite flame retardant comprises the following steps:
Step one, tetraphosphoric acid and ethylene oxide are mixed according to the proportion of 1:5, uniformly mixing and stirring, and reacting for 3 hours under the conditions that the pressure is lower than 0.15MPa and the temperature is 60 ℃ after the replacement of inert gas; after the reaction is finished, aminobenzene with the mass being 2 times of that of ethylene oxide is added into the obtained product components, and the mixture is subjected to heat preservation reaction for 150min at the temperature of 80 ℃ and the pressure of which is lower than 0.15 MPa; after the reaction is finished, the obtained product is a reaction intermediate;
Sequentially adding the modified inorganic substrate and the 2, 6-di-tert-butyl-4-methylphenol into ethanol according to the dosage ratio of 0.004g/mL and 0.005g/mL, uniformly mixing and stirring, placing the obtained mixture into an oil bath pot, heating to 70 ℃ under magnetic stirring, adding an ethanol dispersion liquid of a reaction intermediate with the volume of 5 times and the concentration of 0.008g/mL into the obtained mixed phase, uniformly dispersing, and then carrying out heat preservation reaction for 40h under the protection of nitrogen; and after the reaction is finished, evaporating ethanol in the components of the obtained product, and vacuum drying the obtained solid product at the temperature of 90 ℃ to constant weight to obtain the composite flame retardant.
The preparation method of the modified inorganic substrate comprises the following steps:
Uniformly dispersing the o-hydroxybenzoic acid in thionyl chloride according to the solid-to-liquid ratio of 0.03g/mL, and stopping the reaction when the reflux reaction is carried out until no irritant gas escapes; then evaporating out the residual thionyl chloride in the reaction system to obtain the modifier;
II, ultrasonically dispersing the pretreated inorganic substrate in chloroform according to a solid-to-liquid ratio of 0.02g/mL, and sequentially adding a modifier with the mass of 60% of the pretreated inorganic substrate and triethylamine with the mass of 5%; after being uniformly mixed, nitrogen is introduced, and stirring reaction is carried out until no irritant gas escapes; and filtering the obtained product components, alternately washing the obtained filter cake with chloroform and ethanol for 3 times, and performing vacuum drying treatment to obtain the modified inorganic substrate.
The preparation method of the pretreated inorganic substrate comprises the following steps: uniformly dispersing an inorganic substrate in N, N-dimethylformamide according to a solid-to-liquid ratio of 0.01g/mL, then adding 3-aminopropyl trimethoxysilane with the mass being 30% of that of the inorganic substrate into the N, N-dimethylformamide, uniformly mixing and stirring, and then carrying out reflux reaction for 12h; and after the reaction is finished, carrying out solid-liquid separation on the obtained product components, and sequentially carrying out water washing and vacuum drying treatment on the obtained filter cake to obtain the pretreated inorganic substrate.
The preparation method of the inorganic substrate comprises the following steps: adding ethylene glycol with the mass of 35% of the magnesium nitrate aqueous solution into the magnesium nitrate aqueous solution with the mass of 2mol/L, mixing and stirring uniformly, slowly dripping potassium hydroxide aqueous solution with the same volume and the concentration of 4mol/L into the obtained mixed solution, stirring and reacting for 30 hours at the speed of 2000r/min, aging the obtained precipitate product for 6 hours after the reaction is finished, filtering, washing the obtained filter cake with deionized water until no nitrate ions are detected, washing with absolute ethyl alcohol for 3 times, and vacuum drying the solid powder obtained after washing at the temperature of 100 ℃ until the weight is constant, thus obtaining the inorganic substrate.
The comparative example 1, the present example and the example 1 differ in that: in this example, an equivalent amount of modified inorganic substrate was used in place of the composite flame retardant.
The comparative example 2, the present example and the example 1 are different in that: in this example, the same amount of inorganic substrate was used instead of the composite flame retardant.
Comparative example 3, this example differs from example 1 in that: in this example, the modified inorganic substrate was replaced with an inorganic substrate, i.e., the preparation process of the modified inorganic substrate was omitted, and the inorganic substrate was directly used as a raw material for preparing the composite flame retardant.
Performance test: the following tests were carried out on the relevant properties of the high-strength flame-retardant PC material samples provided in examples 1 to 3 and comparative examples 1 to 3, respectively:
1. Mechanical property test: the tensile properties test was carried out according to ISO527 with a test apparatus of Zwick Z010 electronic tensile machine, germany, with a tensile speed of 50mm/min. The bending performance test was performed in accordance with ISO178, the test equipment being a Zwick Z010 electronic tensile machine, the span being 64mm, the speed being 2mm/min.
2. Flame retardant performance test: limiting Oxygen Index (LOI) is the lowest oxygen concentration that will sustain combustion of a sample in a particular experimental environment and is tested using the method specified in standard GB 2406-93. The vertical burn test (UL-94) was carried out according to the method prescribed in the standard GB/T2408-1996.
3. Ageing resistance: according to the GB/T16422.2-2014 plastic laboratory light source exposure test method, placing the plastic laboratory light source exposure test method into a xenon lamp exposure photoyellowing test box for irradiation, and then according to the HG/T3862-2006 plastic yellow index test method, measuring the yellow index to obtain the yellowing index delta YI. The yellowing index delta YI is an important index for representing photo-oxidative aging performance, and the smaller the delta YI is, the better the light yellowing resistance is.
The test data obtained above are recorded in the following table:
As can be seen from comparison and analysis of the related data in the table, the PC material produced by the invention not only has better mechanical properties, but also has excellent ageing resistance and flame retardance, thereby effectively prolonging the service life and guaranteeing the quality. Therefore, the high-strength flame-retardant PC material and the production process thereof provided by the invention have wider market prospect and are more suitable for popularization.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (10)
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