CN114685890A - Functionalized montmorillonite flame-retardant modified polypropylene composite board and preparation method thereof - Google Patents
Functionalized montmorillonite flame-retardant modified polypropylene composite board and preparation method thereof Download PDFInfo
- Publication number
- CN114685890A CN114685890A CN202111557340.0A CN202111557340A CN114685890A CN 114685890 A CN114685890 A CN 114685890A CN 202111557340 A CN202111557340 A CN 202111557340A CN 114685890 A CN114685890 A CN 114685890A
- Authority
- CN
- China
- Prior art keywords
- montmorillonite
- composite board
- flame
- modified polypropylene
- functionalized
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/101—Esters; Ether-esters of monocarboxylic acids
- C08K5/103—Esters; Ether-esters of monocarboxylic acids with polyalcohols
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
- C08K5/134—Phenols containing ester groups
- C08K5/1345—Carboxylic esters of phenolcarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Fireproofing Substances (AREA)
Abstract
The invention relates to the technical field of new materials, and discloses a functionalized montmorillonite flame-retardant modified polypropylene composite board, wherein aminated montmorillonite reacts with imidazole-4-acetic acid to obtain imidazolyl montmorillonite, the imidazolyl montmorillonite reacts with 5, 5-dimethyl-2-chloro-1, 3, 2-dioxaphospho-caprolactoyl phosphate to obtain imidazolinyl ester montmorillonite, the imidazolinyl ester montmorillonite is mixed with polypropylene, and the mixture is pressed by a flat vulcanizing machine to obtain the functionalized montmorillonite flame-retardant modified polypropylene composite board, the attapulgite can absorb and disperse stress, the mechanical property of the composite board is improved, a large amount of oxyacid of phosphorus, nitrogen, ammonia gas and the like can be generated after the imidazolinyl ester is combusted, on one hand, a polypropylene matrix is promoted to form carbon layers, on the other hand, the oxygen concentration around the composite board is reduced, the composite board is prevented from being further combusted, and the montmorillonite can be attached to the surface of the carbon layer, so that the flame retardant effect of the carbon layer is further enhanced, and the flame retardant property of the composite polypropylene plate is improved.
Description
Technical Field
The invention relates to the technical field of new materials, in particular to a functionalized montmorillonite flame-retardant modified polypropylene composite board and a preparation method thereof.
Background
Polypropylene is one of five general-purpose resins, and has certain application in various aspects of daily life such as automobiles, electric wires, buildings and the like, a polypropylene plate prepared by using polypropylene as a matrix has the characteristics of light weight, no toxicity, excellent heat resistance and the like, so the polypropylene plate is favored by consumers in the field of building decoration, but the polypropylene matrix has the obvious defects of low strength, poor impact toughness and flame resistance and the like, and greatly limits the further application and development of the polypropylene plate.
Montmorillonite is a clay mineral with a special chain lamellar structure, is widely applied to industries such as petroleum, chemical engineering, building, papermaking and the like, is used as a functional additive and is filled in an organic polymer material matrix, the excellent performance of montmorillonite is utilized to improve the mechanical, flame retardant and other performances of the organic polymer material, and is a research hotspot in recent years, Chinese patents such as CN106566166A and the like disclose that montmorillonite is used for modifying polypropylene to enhance the comprehensive performances of polypropylene such as stretching, impact resistance and the like to a certain extent, but most of the patents do not modify montmorillonite, so that montmorillonite is easy to agglomerate in the polymer material matrix, and further the final modification effect is not ideal, therefore, montmorillonite is required to be modified, molecules with flame retardant and other functions are further introduced through hydroxyl on the surface of montmorillonite, the functionality of the organic polymer material is enhanced, and the dispersibility of the organic polymer material is improved to a certain extent, so that the organic polymer material is further applied to the field of modification of organic polymer materials.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a functionalized montmorillonite flame-retardant modified polypropylene composite board and a preparation method thereof, and solves the problems of poor impact strength and flame retardant property of the polypropylene board.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: a functionalized montmorillonite flame-retardant modified polypropylene composite board is prepared by the following steps:
(1) adding a toluene solvent, deionized water, montmorillonite and 3-aminopropyltriethoxysilane in a mass ratio of 150-;
(2) adding a dichloromethane solvent and aminated montmorillonite into a reactor, carrying out ultrasonic dispersion for 20-40min, then continuously adding imidazole-4-acetic acid, 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and a catalyst, uniformly mixing, transferring to an oil bath pot, stirring and reacting at 20-40 ℃ for 12-24h, and carrying out suction filtration, washing and drying after the reaction is finished to obtain imidazolyl montmorillonite;
(3) adding a dichloromethane solvent and imidazolyl montmorillonite into a reactor, carrying out ultrasonic dispersion until the dichloromethane solvent and the imidazolyl montmorillonite are completely dissolved, continuously adding 5, 5-dimethyl-2-chloro-1, 3, 2-dioxaphosphorinanyl phosphate and triethylamine, uniformly mixing, transferring to an oil bath pot for reaction, and carrying out suction filtration, washing and drying after the reaction is finished to obtain imidazolinyl ester montmorillonite;
(4) adding polypropylene, imidazoline ester montmorillonite, 0.2-1% of plasticizer triacetin and 0.5-2% of antioxidant 1010 into a high-speed stirrer, uniformly mixing, transferring to a double-screw extruder for granulation, and pressing by a flat vulcanizing machine to obtain the functionalized montmorillonite flame-retardant modified polypropylene composite board.
Preferably, the mass ratio of the dichloromethane solvent, the aminated montmorillonite, the imidazole-4-acetic acid, the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and the catalyst in the step (2) is 350-900:10:3.5-8:6-15: 0.2-0.6.
Preferably, the catalyst in the step (2) is 4-dimethylaminopyridine or 1-hydroxybenzotriazole.
Preferably, the mass ratio of the dichloromethane solvent, the imidazolyl montmorillonite, the 5, 5-dimethyl-2-chloro-1, 3, 2-dioxaphosphorinanyl phosphate and the triethylamine in the step (3) is 300-850:10:2.5-6: 3-7.5.
Preferably, the reaction temperature in the step (3) is 15-35 ℃ and the reaction time is 6-12 h.
Preferably, the mass ratio of the polypropylene to the imidazolinyl montmorillonite in the step (4) is 100: 2.5-6.
(III) advantageous technical effects
Compared with the prior art, the invention has the following beneficial technical effects:
the functionalized montmorillonite flame-retardant modified polypropylene composite board is characterized in that the surface of montmorillonite is rich in hydroxyl, the aminated montmorillonite is obtained after being modified by 3-aminopropyltriethoxysilane, under the action of a catalyst 4-dimethylaminopyridine and a dehydrating agent 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, the amino group of the aminated montmorillonite can perform amidation reaction with the carboxyl group in imidazole-4-acetic acid to obtain imidazolyl montmorillonite, under the action of an acid-binding agent triethylamine, the imino group of the imidazole group in the imidazolyl montmorillonite can perform phosphoric acid amidation reaction with the phosphorus oxychloride group in a 5, 5-dimethyl-2-chlorine-1, 3, 2-dioxaphosphorinane phosphate ester structure to obtain imidazolinyl ester montmorillonite, so that the imidazoline ester montmorillonite is obtained through the connection mode of chemical bonds, the nitrogen-phosphorus synergistic flame retardant is covalently grafted on the surface of the montmorillonite, so that the surface modification of the montmorillonite is realized, and the functionality of the montmorillonite is enriched, thereby effectively expanding the application range of the montmorillonite.
The functionalized montmorillonite flame-retardant modified polypropylene composite board is prepared by blending polypropylene, imidazoline ester montmorillonite and various auxiliaries, pressing the mixture by a press vulcanizer to obtain the functionalized montmorillonite flame-retardant modified polypropylene composite board, wherein the montmorillonite and the polypropylene matrix which are organically treated on the surface have a good interface effect, the dispersity of the montmorillonite in the polypropylene matrix is improved to a certain extent, when the composite board is subjected to external force, stress is transferred to the montmorillonite from the polypropylene matrix, the yield and plastic deformation of the polypropylene matrix are effectively promoted, so that the composite board system absorbs more energy, and meanwhile, microcracks generated by the stress are hindered by the montmorillonite in the process of expansion, so that the cracks are terminated, turned or deflected, so that the fracture aspect is increased, and a large amount of stress energy is absorbed, the properties of the composite polypropylene plate such as toughness, impact strength and the like are effectively improved, the dioxacaprolactoyl imidazolyl group grafted on the surface of the montmorillonite is used as a nitrogen-phosphorus synergistic flame retardant, when the composite plate burns, a large amount of oxyacid, nitrogen, ammonia and the like of phosphorus can be generated, on one hand, the polypropylene matrix is promoted to form carbon to form a carbon layer to protect the inside of the matrix, on the other hand, the oxygen concentration around the composite plate is reduced, the composite plate is prevented from further burning, and combustion products of the montmorillonite such as magnesium-aluminum silicate and the like can be attached to the surface of the carbon layer to further enhance the flame retardant effect of the carbon layer, so that the flame retardant property of the composite polypropylene plate is effectively improved.
Drawings
FIG. 1 is a schematic representation of the reaction of an aminated montmorillonite with imidazole-4-acetic acid.
FIG. 2 is a schematic representation of the reaction of imidazolyl montmorillonite with 5, 5-dimethyl-2-chloro-1, 3, 2-dioxaphosphorinanyl phosphate.
FIG. 3 is a graph showing impact strength tests of the composite sheets in examples and comparative examples.
Fig. 4 is a heat release rate test chart of the composite sheets in examples and comparative examples.
Detailed Description
To achieve the above object, the present invention provides the following embodiments: a preparation method of a functionalized montmorillonite flame-retardant modified polypropylene composite board comprises the following steps:
example 1
(1) Adding 90mL of toluene solvent, 25mL of deionized water, 5g of montmorillonite and 0.025g of 3-aminopropyltriethoxysilane into a reactor, uniformly mixing, stirring and reacting for 2 hours in an oil bath kettle at a constant temperature of 70 ℃, and performing suction filtration, washing and drying after the reaction is finished to obtain aminated montmorillonite;
(2) adding 135mL of dichloromethane solvent and 5g of aminated montmorillonite into a reactor, carrying out ultrasonic dispersion for 20min, then continuously adding 1.75g of imidazole-4-acetic acid, 0.1g of 4-dimethylaminopyridine and 3g of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, uniformly mixing, transferring into an oil bath pot, carrying out stirring reaction at 20 ℃ for 12h, carrying out suction filtration, washing and drying after the reaction is finished, and thus obtaining imidazolyl montmorillonite;
(3) adding 120mL of dichloromethane solvent and 5g of azolyl montmorillonite into a reactor, carrying out ultrasonic dispersion until the dichloromethane solvent and the azolyl montmorillonite are completely dissolved, continuing adding 1.25g of 5, 5-dimethyl-2-chloro-1, 3, 2-dioxaphosphorinane phosphate and 1.5g of triethylamine, uniformly mixing, transferring to an oil bath pot, reacting for 6 hours at 15 ℃, carrying out suction filtration, washing and drying after the reaction is finished, and obtaining imidazoline ester group montmorillonite;
(4) adding 50g of polypropylene, 1.25g of imidazoline ester montmorillonite, 0.1g of plasticizer triacetin and 0.25g of antioxidant 1010 into a high-speed stirrer, uniformly mixing, transferring the mixture to a double-screw extruder for granulation, and pressing the mixture by a flat vulcanizing machine to obtain the functionalized montmorillonite flame-retardant modified polypropylene composite board.
Example 2
(1) Adding 100mL of toluene solvent, 30mL of deionized water, 5g of montmorillonite and 0.035g of 3-aminopropyltriethoxysilane into a reactor, uniformly mixing, stirring and reacting for 3 hours in an oil bath kettle at a constant temperature of 75 ℃, and performing suction filtration, washing and drying after the reaction is finished to obtain aminated montmorillonite;
(2) adding 180mL of dichloromethane solvent and 5g of aminated montmorillonite into a reactor, carrying out ultrasonic dispersion for 25min, then continuously adding 2.2g of imidazole-4-acetic acid, 0.15g of 1-hydroxybenzotriazole and 4g of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, uniformly mixing, transferring into an oil bath pot, carrying out stirring reaction at 25 ℃ for 16h, carrying out suction filtration, washing and drying after the reaction is finished, thus obtaining imidazolyl montmorillonite;
(3) adding 160mL of dichloromethane solvent and 5g of azolyl montmorillonite into a reactor, carrying out ultrasonic dispersion until the dichloromethane solvent and the azolyl montmorillonite are completely dissolved, continuing adding 1.8g of 5, 5-dimethyl-2-chloro-1, 3, 2-dioxaphosphorinane phosphate and 2.5g of triethylamine, uniformly mixing, transferring to an oil bath pot, reacting for 8 hours at 20 ℃, carrying out suction filtration, washing and drying after the reaction is finished, and obtaining imidazoline ester group montmorillonite;
(4) adding 50g of polypropylene, 1.8g of imidazoline ester montmorillonite, 0.2g of plasticizer triacetin and 0.4g of antioxidant 1010 into a high-speed stirrer, uniformly mixing, transferring the mixture to a double-screw extruder for granulation, and pressing the mixture by a flat vulcanizing machine to obtain the functionalized montmorillonite flame-retardant modified polypropylene composite board.
Example 3
(1) Adding 110mL of toluene solvent, 35mL of deionized water, 5g of montmorillonite and 0.045g of 3-aminopropyltriethoxysilane into a reactor, uniformly mixing, stirring and reacting for 4 hours in an oil bath kettle at a constant temperature of 80 ℃, and performing suction filtration, washing and drying after the reaction is finished to obtain aminated montmorillonite;
(2) adding 240mL of dichloromethane solvent and 5g of aminated montmorillonite into a reactor, carrying out ultrasonic dispersion for 30min, then continuously adding 2.8g of imidazole-4-acetic acid, 0.2g of 4-dimethylaminopyridine and 5g of 1- (3-dimethylaminopropyl) -3-ethyl carbodiimide hydrochloride, uniformly mixing, transferring into an oil bath pot, carrying out stirring reaction at 30 ℃ for 18h, carrying out suction filtration, washing and drying after the reaction is finished, thus obtaining imidazolyl montmorillonite;
(3) adding 240mL of dichloromethane solvent and 5g of azolyl montmorillonite into a reactor, carrying out ultrasonic dispersion until the dichloromethane solvent and the azolyl montmorillonite are completely dissolved, continuously adding 2.2g of 5, 5-dimethyl-2-chloro-1, 3, 2-dioxaphosphorinane phosphate and 3g of triethylamine, uniformly mixing, transferring to an oil bath pot, reacting for 9 hours at 25 ℃, carrying out suction filtration, washing and drying after the reaction is finished, and obtaining imidazoline ester group montmorillonite;
(4) adding 50g of polypropylene, 2.2g of imidazoline ester montmorillonite, 0.3g of plasticizer triacetin and 0.6g of antioxidant 1010 into a high-speed stirrer, uniformly mixing, transferring the mixture to a double-screw extruder for granulation, and pressing the mixture by a flat vulcanizing machine to obtain the functionalized montmorillonite flame-retardant modified polypropylene composite board.
Example 4
(1) Adding 120mL of toluene solvent, 40mL of deionized water, 5g of montmorillonite and 0.06g of 3-aminopropyltriethoxysilane into a reactor, uniformly mixing, stirring and reacting for 5 hours in an oil bath kettle at a constant temperature of 85 ℃, and performing suction filtration, washing and drying after the reaction is finished to obtain aminated montmorillonite;
(2) adding 300mL of dichloromethane solvent and 5g of aminated montmorillonite into a reactor, carrying out ultrasonic dispersion for 35min, then continuously adding 3.4g of imidazole-4-acetic acid, 0.25g of 1-hydroxybenzotriazole and 6g of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, uniformly mixing, transferring into an oil bath pot, carrying out stirring reaction at 35 ℃ for 20h, carrying out suction filtration, washing and drying after the reaction is finished, and thus obtaining imidazolyl montmorillonite;
(3) adding 280mL of dichloromethane solvent and 5g of azolyl montmorillonite into a reactor, carrying out ultrasonic dispersion until the dichloromethane solvent and the azolyl montmorillonite are completely dissolved, continuously adding 2.6g of 5, 5-dimethyl-2-chloro-1, 3, 2-dioxaphosphorinane phosphate and 4g of triethylamine, uniformly mixing, transferring to an oil bath pot, reacting for 10 hours at 30 ℃, carrying out suction filtration, washing and drying after the reaction is finished, and obtaining imidazoline ester group montmorillonite;
(4) adding 50g of polypropylene, 2.6g of imidazoline ester montmorillonite, 0.4g of plasticizer triacetin and 0.8g of antioxidant 1010 into a high-speed stirrer, uniformly mixing, transferring the mixture to a double-screw extruder for granulation, and pressing the mixture by a flat vulcanizing machine to obtain the functionalized montmorillonite flame-retardant modified polypropylene composite board.
Example 5
(1) Adding 130mL of toluene solvent, 50mL of deionized water, 5g of montmorillonite and 0.075g of 3-aminopropyltriethoxysilane into a reactor, uniformly mixing, stirring and reacting for 6 hours in an oil bath kettle at a constant temperature of 90 ℃, and performing suction filtration, washing and drying after the reaction is finished to obtain aminated montmorillonite;
(2) adding 330mL of dichloromethane solvent and 5g of aminated montmorillonite into a reactor, carrying out ultrasonic dispersion for 40min, then continuously adding 4g of imidazole-4-acetic acid, 0.3g of 4-dimethylaminopyridine and 7.5g of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, uniformly mixing, transferring into an oil bath pot, carrying out stirring reaction at 40 ℃ for 24h, carrying out suction filtration, washing and drying after the reaction is finished, and thus obtaining imidazolyl montmorillonite;
(3) adding 320mL of dichloromethane solvent and 5g of azolyl montmorillonite into a reactor, carrying out ultrasonic dispersion until the dichloromethane solvent and the azolyl montmorillonite are completely dissolved, continuing adding 3g of 5, 5-dimethyl-2-chloro-1, 3, 2-dioxaphosphorinanyl phosphate and 4.75g of triethylamine, uniformly mixing, transferring to an oil bath pot, reacting for 12 hours at 35 ℃, carrying out suction filtration, washing and drying after the reaction is finished, and obtaining imidazoline ester group montmorillonite;
(4) adding 50g of polypropylene, 3g of imidazoline ester montmorillonite, 0.5g of plasticizer triacetin and 1g of antioxidant 1010 into a high-speed stirrer, uniformly mixing, transferring the mixture to a double-screw extruder for granulation, and pressing the mixture by a flat vulcanizing machine to obtain the functionalized montmorillonite flame-retardant modified polypropylene composite board.
Comparative example 1
(1) Adding 100mL of toluene solvent, 30mL of deionized water, 5g of montmorillonite and 0.03g of 3-aminopropyltriethoxysilane into a reactor, uniformly mixing, stirring and reacting for 2 hours in an oil bath kettle at a constant temperature of 75 ℃, and performing suction filtration, washing and drying after the reaction is finished to obtain aminated montmorillonite;
(2) adding 150mL of dichloromethane solvent and 5g of aminated montmorillonite into a reactor, carrying out ultrasonic dispersion for 20min, then continuously adding 1.8g of imidazole-4-acetic acid, 0.12g of 4-dimethylaminopyridine and 3.5g of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, uniformly mixing, transferring into an oil bath pot, stirring and reacting for 15h at 25 ℃, carrying out suction filtration, washing and drying after the reaction is finished, thus obtaining imidazolyl montmorillonite;
(3) adding 50g of polypropylene, 1.5g of imidazolyl montmorillonite, 0.2g of plasticizer triacetin and 0.3g of antioxidant 1010 into a high-speed stirrer, uniformly mixing, transferring the mixture to a double-screw extruder for granulation, and pressing the mixture by a flat vulcanizing machine to obtain the montmorillonite modified polypropylene composite board.
The composite boards of the examples and comparative examples were injection molded into samples having a specification of 6mm × 8cm × 8cm, and the impact strength was measured using an ASR-XJJ-11B impact strength tester, according to GB/T1043-2008.
The composite boards of examples and comparative examples were injection-molded into samples of 6mm × 8cm × 8cm in specification, wrapped with aluminum foil, padded with ceramic fiber wool at the bottom, placed with a steel grid on the surface and covered, and set to have a heat radiation amount of 30kW/m2The heat release rate was measured using an ME1200-1 heat release rate tester.
Claims (6)
1. A preparation method of a functionalized montmorillonite flame-retardant modified polypropylene composite board is characterized by comprising the following steps:
(1) uniformly mixing a toluene solvent, deionized water, montmorillonite and 3-aminopropyltriethoxysilane in a mass ratio of 150-;
(2) adding aminated montmorillonite into a dichloromethane solvent, performing ultrasonic dispersion for 20-40min, then continuously adding imidazole-4-acetic acid, 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and a catalyst, uniformly mixing, transferring to an oil bath pot, stirring and reacting at 20-40 ℃ for 12-24h, and performing suction filtration, washing and drying after the reaction is finished to obtain imidazolyl montmorillonite;
(3) adding imidazolyl montmorillonite into a dichloromethane solvent, carrying out ultrasonic dispersion until the imidazolyl montmorillonite is completely dissolved, continuously adding 5, 5-dimethyl-2-chloro-1, 3, 2-dioxaphosphorinane phosphate and triethylamine, uniformly mixing, transferring to an oil bath pot for reaction, and carrying out suction filtration, washing and drying after the reaction is finished to obtain imidazolinyl ester montmorillonite;
(4) adding polypropylene, imidazoline ester montmorillonite, 0.2-1% of plasticizer triacetin and 0.5-2% of antioxidant 1010 into a high-speed stirrer, uniformly mixing, transferring to a double-screw extruder for granulation, and pressing by a flat vulcanizing machine to obtain the functionalized montmorillonite flame-retardant modified polypropylene composite board.
2. The preparation method of the functionalized montmorillonite flame-retardant modified polypropylene composite board according to claim 1, characterized by comprising the following steps: the mass ratio of the dichloromethane solvent, the aminated montmorillonite, the imidazole-4-acetic acid, the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and the catalyst in the step (2) is 350-900:10:3.5-8:6-15: 0.2-0.6.
3. The preparation method of the functionalized montmorillonite flame-retardant modified polypropylene composite board according to claim 1, which is characterized by comprising the following steps: the catalyst in the step (2) is 4-dimethylaminopyridine or 1-hydroxybenzotriazole.
4. The preparation method of the functionalized montmorillonite flame-retardant modified polypropylene composite board according to claim 1, which is characterized by comprising the following steps: in the step (3), the mass ratio of the dichloromethane solvent, the imidazolyl montmorillonite, the 5, 5-dimethyl-2-chloro-1, 3, 2-dioxaphosphorinanyl phosphate and the triethylamine is 300-850:10:2.5-6: 3-7.5.
5. The preparation method of the functionalized montmorillonite flame-retardant modified polypropylene composite board according to claim 1, which is characterized by comprising the following steps: the reaction temperature in the step (3) is 15-35 ℃, and the reaction time is 6-12 h.
6. The preparation method of the functionalized montmorillonite flame-retardant modified polypropylene composite board according to claim 1, which is characterized by comprising the following steps: the mass ratio of the polypropylene to the imidazoline ester montmorillonite in the step (4) is 100: 2.5-6.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111557340.0A CN114685890B (en) | 2021-12-19 | 2021-12-19 | Functionalized montmorillonite flame-retardant modified polypropylene composite board and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111557340.0A CN114685890B (en) | 2021-12-19 | 2021-12-19 | Functionalized montmorillonite flame-retardant modified polypropylene composite board and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114685890A true CN114685890A (en) | 2022-07-01 |
| CN114685890B CN114685890B (en) | 2023-09-12 |
Family
ID=82136179
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111557340.0A Active CN114685890B (en) | 2021-12-19 | 2021-12-19 | Functionalized montmorillonite flame-retardant modified polypropylene composite board and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114685890B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116589777A (en) * | 2023-06-16 | 2023-08-15 | 高尚蓉 | Halogen-free flame-retardant crosslinked polyethylene cable material and preparation method thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014100923A1 (en) * | 2012-12-31 | 2014-07-03 | 中国科学院化学研究所 | Clay-enhanced polypropylene intra-autoclave alloy, preparation method for same, and applications thereof |
| CN108997649A (en) * | 2018-06-22 | 2018-12-14 | 宁波蒙曼生物科技有限公司 | A kind of anti-flaming polypropylene material and its preparation and application |
| CN110437354A (en) * | 2019-07-05 | 2019-11-12 | 深圳聚石新材料科技有限公司 | Ultra-high molecular weight polyethylene/Nano composite material of montmorillonite preparation method |
| WO2021128102A1 (en) * | 2019-12-25 | 2021-07-01 | 宁波禾隆新材料股份有限公司 | Flame-retardant wood-plastic surface layer composite, and method for preparing wood-plastic composite material having flame-retardant wood-plastic surface composite |
| CN113373536A (en) * | 2021-06-29 | 2021-09-10 | 南陵县麒霆新材料科技有限公司 | Functionalized modified silicon dioxide flame-retardant modified polylactic acid composite fiber and preparation method thereof |
| CN113372813A (en) * | 2021-05-17 | 2021-09-10 | 上海电力大学 | Preparation method of montmorillonite/sol-gel composite coating |
| CN113737303A (en) * | 2021-09-22 | 2021-12-03 | 武汉迷思迈纺织有限公司 | Organic montmorillonite toughened and modified PET anti-ultraviolet aging fiber and preparation method thereof |
-
2021
- 2021-12-19 CN CN202111557340.0A patent/CN114685890B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014100923A1 (en) * | 2012-12-31 | 2014-07-03 | 中国科学院化学研究所 | Clay-enhanced polypropylene intra-autoclave alloy, preparation method for same, and applications thereof |
| CN108997649A (en) * | 2018-06-22 | 2018-12-14 | 宁波蒙曼生物科技有限公司 | A kind of anti-flaming polypropylene material and its preparation and application |
| CN110437354A (en) * | 2019-07-05 | 2019-11-12 | 深圳聚石新材料科技有限公司 | Ultra-high molecular weight polyethylene/Nano composite material of montmorillonite preparation method |
| WO2021128102A1 (en) * | 2019-12-25 | 2021-07-01 | 宁波禾隆新材料股份有限公司 | Flame-retardant wood-plastic surface layer composite, and method for preparing wood-plastic composite material having flame-retardant wood-plastic surface composite |
| CN113372813A (en) * | 2021-05-17 | 2021-09-10 | 上海电力大学 | Preparation method of montmorillonite/sol-gel composite coating |
| CN113373536A (en) * | 2021-06-29 | 2021-09-10 | 南陵县麒霆新材料科技有限公司 | Functionalized modified silicon dioxide flame-retardant modified polylactic acid composite fiber and preparation method thereof |
| CN113737303A (en) * | 2021-09-22 | 2021-12-03 | 武汉迷思迈纺织有限公司 | Organic montmorillonite toughened and modified PET anti-ultraviolet aging fiber and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 张立飞;柳军旺;马成国;王永亮;韩志东;: "氢氧化镁/可膨胀石墨/聚丙烯复合材料的热降解过程与燃烧行为", 华南师范大学学报(自然科学版), no. 01 * |
| 覃善丽;: "阻燃剂的改性研究进展", 大众科技, no. 05 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116589777A (en) * | 2023-06-16 | 2023-08-15 | 高尚蓉 | Halogen-free flame-retardant crosslinked polyethylene cable material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114685890B (en) | 2023-09-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Xu et al. | Constructing SiO2 nanohybrid to develop a strong soy protein adhesive with excellent flame-retardant and coating ability | |
| CN106750550B (en) | A kind of fire retardant elastic nano-cellulose aerogel and preparation method thereof | |
| CN102174247A (en) | Halogen-free flame retardant glass fiber reinforced polyester composite and preparation method thereof | |
| CN113278191A (en) | Aramid nanofiber-based composite aerogel and preparation method thereof | |
| CN114685890A (en) | Functionalized montmorillonite flame-retardant modified polypropylene composite board and preparation method thereof | |
| CN109705634B (en) | Attapulgite-based composite flame retardant modified by nitrogen-phosphorus-containing organic matter and preparation and application thereof | |
| FI95727C (en) | Highly flammable, high temperature resistant polyimide fibers and moldings made therefrom | |
| CN108164751B (en) | Reactive halogen-free flame retardant suitable for TPV (thermoplastic vulcanizate), and preparation method and application thereof | |
| CN113121885B (en) | Flame retardant, flame-retardant PLA composite material and preparation method thereof | |
| NL2030477B1 (en) | Underwater Elastic Cellulose Aerogel and Preparation Method and Application Thereof | |
| CN112175378A (en) | Preparation method of environment-friendly wear-resistant high polymer material | |
| CN109438759B (en) | Nitrogen-phosphorus composite intercalation modified zirconium phosphate with flame retardant effect and preparation method thereof | |
| CN108586807B (en) | Flame-retardant functionalized graphene and preparation and application thereof | |
| CN114196129A (en) | Nitrogen-phosphorus synergistic flame-retardant functionalized montmorillonite modified PVC wood-plastic plate and preparation method thereof | |
| CN114213759B (en) | Preparation method and application of polyphosphonate grafted graphene flame-retardant modified polypropylene | |
| CN112759301B (en) | Environment-friendly warm mix asphalt mixture | |
| CN114292508A (en) | Functional nano zinc oxide modified polycarbonate sheet and preparation method thereof | |
| Zhang et al. | Flame retardant cellulose/polyvinyl alcohol/sodium alginate composite aerogels crosslinked by metal ions for flame resistance materials | |
| CN104829832A (en) | Preparation method of organic-silicone-modified flame-retarding nylon-6 | |
| CN112442895A (en) | Chelate coordination type phosphorus-boron-nitrogen synergistic flame retardant and preparation method thereof | |
| CN113388351A (en) | Multifunctional modified epoxy resin adhesive and preparation method thereof | |
| CN110903442B (en) | Flame-retardant modified corn straw and preparation method thereof | |
| CN114479079B (en) | Polyimide aerogel and preparation method thereof | |
| CN112029157B (en) | Anti-dripping composite intumescent flame retardant and preparation method and application thereof | |
| CN114874541A (en) | Flame-retardant smoke-suppressing polymer composite material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |