CN110746761A - High-strength heat-resistant flame-retardant heat-insulating material - Google Patents

High-strength heat-resistant flame-retardant heat-insulating material Download PDF

Info

Publication number
CN110746761A
CN110746761A CN201911181022.1A CN201911181022A CN110746761A CN 110746761 A CN110746761 A CN 110746761A CN 201911181022 A CN201911181022 A CN 201911181022A CN 110746761 A CN110746761 A CN 110746761A
Authority
CN
China
Prior art keywords
parts
powder
heat
resistant
resistant flame
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.)
Pending
Application number
CN201911181022.1A
Other languages
Chinese (zh)
Inventor
艾明生
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
HEXIAN MINGSHENG ENVIRONMENTAL PROTECTION MATERIAL Co Ltd
Original Assignee
HEXIAN MINGSHENG ENVIRONMENTAL PROTECTION MATERIAL Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by HEXIAN MINGSHENG ENVIRONMENTAL PROTECTION MATERIAL Co Ltd filed Critical HEXIAN MINGSHENG ENVIRONMENTAL PROTECTION MATERIAL Co Ltd
Priority to CN201911181022.1A priority Critical patent/CN110746761A/en
Publication of CN110746761A publication Critical patent/CN110746761A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/06Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
    • C08J9/10Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
    • C08J9/104Hydrazines; Hydrazides; Semicarbazides; Semicarbazones; Hydrazones; Derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0014Use of organic additives
    • C08J9/0028Use of organic additives containing nitrogen
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0061Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0066Use of inorganic compounding ingredients
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0095Mixtures of at least two compounding ingredients belonging to different one-dot groups
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/06Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
    • C08J9/10Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
    • C08J9/102Azo-compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/06Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
    • C08J9/10Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
    • C08J9/104Hydrazines; Hydrazides; Semicarbazides; Semicarbazones; Hydrazones; Derivatives thereof
    • C08J9/105Hydrazines; Hydrazides; Semicarbazides; Semicarbazones; Hydrazones; Derivatives thereof containing sulfur
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2203/00Foams characterized by the expanding agent
    • C08J2203/04N2 releasing, ex azodicarbonamide or nitroso compound
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2371/00Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
    • C08J2371/08Polyethers derived from hydroxy compounds or from their metallic derivatives
    • C08J2371/10Polyethers derived from hydroxy compounds or from their metallic derivatives from phenols
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2483/00Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
    • C08J2483/16Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers in which all the silicon atoms are connected by linkages other than oxygen atoms
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2485/00Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon; Derivatives of such polymers
    • C08J2485/02Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon; Derivatives of such polymers containing phosphorus

Abstract

The invention discloses a high-strength heat-resistant flame-retardant heat-insulating material which is prepared from the following raw materials: 23-45 parts of poly (arylene ether nitrile), 33-54 parts of polyimide, 11-17 parts of fluorinated phosphazene rubber, 7-13 parts of phthalonitrile, 3-7 parts of chromite powder, 2-5 parts of cordierite powder, 3-6 parts of 4,4' -diaminodiphenylmethane, 4-7 parts of cyanite powder, 0.5-1 part of curing agent, 5-8 parts of polycarbosilane, 3-6 parts of magnesium aluminate spinel powder, 1-2 parts of lanthanum hexaboride, 1-1.5 parts of foaming agent and 45-68 parts of methanol. The high-strength heat-resistant flame-retardant heat-insulating material disclosed by the invention is light in weight, high in surface energy, strong in impurity phase adsorption capacity, excellent in thermal shock resistance, noise-reducing and insulating, high in strength, free of slag falling, wear-resistant, impact-resistant, low in water absorption, fireproof, heat-resistant, radiation-resistant, drop-resistant, non-toxic and environment-friendly, can be used for a long time under extreme conditions of ultrahigh temperature, ultralow temperature, high salt spray, strong noise, strong corrosion, strong radiation and the like, and has extremely high reliability and quality guarantee.

Description

High-strength heat-resistant flame-retardant heat-insulating material
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a high-strength heat-resistant flame-retardant heat-insulating material.
Background
The polyimide foam is used as the most elegant heat-insulating and sound-insulating material and is applied to the fields of aerospace and aviation of various countries and the basic configuration of high-end buildings on ships and high-end buildings of American military ships. The material has the characteristics of excellent comprehensive performance of intrinsic flame retardance, environmental protection, no toxicity, wide temperature tolerance range, low thermal conductivity, irradiation resistance, light weight, easy processing and installation and the like, can be used for a long time under extreme conditions of ultrahigh temperature, ultralow temperature, high salt spray, strong noise, strong corrosion, strong radiation and the like, and has extremely high reliability and quality guarantee.
The existing ship uses rock wool as heat-insulating noise-reducing material, its weight is 10-30 times that of polyimide foam, and its weight is high, it is easy to absorb water and lose efficacy, and its service cycle is short. Rockwool is used because it is not made domestically and is too expensive. With the development of the aerospace and navigation industries, the demand of polyimide foam products in China is rapidly increased, and a large amount of high-end polyimide foam products are urgently needed in the fields of advanced military equipment, building heat preservation and the like.
On the other hand, along with the occurrence of several extra-large fires in the industry of external wall insulation materials of civil buildings in China, the fire protection safety of the external wall insulation materials is emphasized, and the insulation foam materials with good fireproof performance and moderate price are urgently needed. High performance polyimide foam is a suitable choice, but the toughness is poor, and the foaming process is complex. The development of a novel high-light heat-resistant flame-retardant heat-insulating material is urgently needed by the technical personnel in the field.
Disclosure of Invention
The invention aims to provide a high-strength heat-resistant flame-retardant heat-insulating material aiming at the existing problems.
The invention is realized by the following technical scheme:
a high-strength heat-resistant flame-retardant heat-insulation material is prepared from the following raw materials in parts by weight: 23-45 parts of poly (arylene ether nitrile), 33-54 parts of ketone anhydride, 11-17 parts of fluorinated phosphazene rubber, 7-13 parts of phthalonitrile, 3-7 parts of chromite powder, 2-5 parts of cordierite powder, 3-6 parts of 4,4' -diaminodiphenylmethane, 4-7 parts of cyanite powder, 0.5-1 part of curing agent, 5-8 parts of polycarbosilane, 3-6 parts of magnesium aluminate spinel powder, 1-2 parts of lanthanum hexaboride, 1-1.5 parts of foaming agent and 45-68 parts of methanol.
Further, the fluoroether rubber is binary copolymerization fluoroether rubber, and the fluorine content of the fluoroether rubber is 24-37%.
Further, the curing agent is a mixture of bis- [ gamma- (triethoxy silicon) propyl ] tetrasulfide, dicyandiamide and sebacic dihydrazide, and the proportion of the curing agent is 1-2: 2-4: 3-5.
Further, the foaming agent is one or more of trihydrazinotriazine, 4' -oxybis (benzenesulfonylamino urea) and barium azodicarboxylate.
Further, the polycarbosilane is allyl hydrogenated polycarbosilane.
A preparation method of a high-strength heat-resistant flame-retardant heat-insulating material comprises the following steps:
(1) preparing raw materials according to the weight percentage; (2) synthesizing a polyesteramide prepolymer, mixing half of total amount of ketonic anhydride and half of total amount of methanol, stirring at 50 ℃ for reaction for esterification, adding 4,4' -diaminodiphenylmethane to obtain a polyesteramide prepolymer solution, and drying to obtain polyesteramide prepolymer powder; adding the residual ketonic anhydride into the residual methanol at room temperature, heating, condensing, refluxing until the solution is transparent, pouring the solution into a stainless steel container, stirring for a certain time to obtain a polyesteramide prepolymer solution, cooling to room temperature, pouring the polyesteramide prepolymer mixed solution into a reaction kettle, putting the reaction kettle into a vacuum drying oven, vacuumizing to-0.1 MPa, keeping the temperature at 50-60 ℃ for 24 hours, taking out, and milling to obtain light yellow polyesteramide prepolymer powder; (3) uniformly mixing polyamide ester prepolymer powder, poly (arylene ether nitrile), phosphonitrile fluoride rubber, phthalonitrile, chromite powder, cordierite powder, kyanite powder, a regulator, polycarbosilane, magnesium-aluminum spinel powder and lanthanum hexaboride, adding the mixture into a mold, placing the mold into a 2450-2500 MHZ microwave oven, keeping the mold for 0.5-1 min, then placing the mold into a muffle furnace at 280 ℃, introducing nitrogen as a protective gas, keeping the mold for 10-30 min, raising the temperature of the muffle furnace to 310 ℃, and keeping the temperature for 20-40 min; (4) and pouring out the viscous mixture in the die, melting and plasticizing at 310-350 ℃ in a double-screw extruder, mixing a curing agent and a foaming agent during the process, quenching to below 50 ℃ by taking nitrogen as protective gas, introducing supercritical carbon dioxide, carrying out saturated adsorption, wherein the saturated adsorption pressure is 42-50 MPa, the saturated adsorption time is 28-30 h, the saturated adsorption temperature is-5-25 ℃, releasing pressure from the supercritical carbon dioxide, taking out, rapidly placing in an oil bath at 240-350 ℃ for foaming for 1-2min, quenching in distilled water at room temperature after foaming is finished, cleaning and shaping, and carrying out vacuum drying to obtain the high-strength heat-resistant flame-retardant heat-insulating material.
The invention has the beneficial effects that:
according to the invention, the two-step foaming agent and the supercritical carbon dioxide foaming source are adopted, so that the foaming rate and the size of the foam holes can be reasonably controlled, the strength of the material is further improved, the polyimide, the polyarylethernitrile and the fluoroether rubber are blended and modified, the obtained foam material has uniform foam holes, high strength, good flame retardance, high temperature resistance and good sound insulation and sound absorption in the sound wave frequency range of 0-2000 Hz. The curing and foaming speeds of the resin can be well controlled, the hardness of the cured resin and the matching of the poly (arylene ether nitrile) are good, an IPN foam material with increased compression strength and compression modulus is formed, the impact strength is reduced, the poly (arylene ether nitrile) and polyimide in the IPN foam material are good in compatibility, the damping performance is high, and good damping behavior is shown. Interpenetrating network polymers (IPNs) are a new class of polymer alloys consisting of two or more crosslinked polymers. The attachment of a small number of covalent bonds between polymers forms a permanent entanglement of the network, and IPNs therefore exhibit some particular macromolecular topographies. The connection of the polyimide, the polyaryl ether nitrile and other components can obtain good synergistic effect, and the connection contains the main chain structure of the polyaryl ether nitrile molecules and also contains a fluoroether rubber structure. Therefore, the heat resistance and mechanical strength of polyimide and polyarylene ether nitrile are improved, and the toughness and impact resistance of the fluoroether rubber are improved. The introduction of phthalonitrile and lanthanum hexaboride further improves the crosslinking density, makes the crosslinking bonding more compact and further improves the material strength. The addition of the chromium quartz powder, the cordierite powder, the sapphire powder and the magnesium aluminate spinel powder not only reduces the cost of the material, but also improves the corrosion resistance, the fire resistance and the heat resistance of the material, and has good flame retardant effect without adding extra flame retardant. The introduction of the fluoroether rubber further improves the compatibility among the material components and the impact resistance and corrosion resistance of the material. The reasonable foaming system and the curing system not only improve the heat insulation performance of the material, but also provide a plurality of crosslinking key joint modes, further improve the crosslinking density and further improve the strength and the heat resistance of the material.
Compared with the prior art, the invention has the following advantages:
the high-strength heat-resistant flame-retardant heat-insulating material disclosed by the invention has the advantages of high aperture ratio, light weight, high surface energy, strong impurity phase adsorption force, excellent thermal shock resistance, noise reduction, insulation, high strength, no slag falling, wear resistance, impact resistance, low water absorption, fire resistance, heat resistance, radiation resistance, falling resistance, no toxicity, environmental friendliness, capability of being used for a long time under extreme conditions of ultrahigh temperature, ultralow temperature, high salt mist, strong noise, strong corrosion, strong radiation and the like, and extremely high reliability and quality guarantee.
Detailed Description
The invention is illustrated by the following specific examples, which are not intended to be limiting.
Example 1
A high-strength heat-resistant flame-retardant heat-insulation material is prepared from the following raw materials in parts by weight: 45 parts of poly (arylene ether nitrile), 54 parts of ketone anhydride, 17 parts of fluorinated phosphazene rubber, 13 parts of phthalonitrile, 7 parts of chromolite powder, 5 parts of cordierite powder, 6 parts of 4,4' -diaminodiphenylmethane, 7 parts of cyanite powder, 1 part of curing agent, 8 parts of polycarbosilane, 6 parts of magnesium aluminate spinel powder, 2 parts of lanthanum hexaboride, 1 part of foaming agent and 68 parts of methanol.
Further, the fluoroether rubber is binary copolymerization fluoroether rubber, and the fluorine content of the fluoroether rubber is 24-37%.
Further, the curing agent is a mixture of bis- [ gamma- (triethoxy silicon) propyl ] tetrasulfide, dicyandiamide and sebacic dihydrazide, and the proportion of the curing agent is 1: 2: 3.
Further, the foaming agent is trihydrazinotriazine, 4' -oxybis (benzenesulfonylamino urea) and barium azodicarboxylate.
Further, the polycarbosilane is allyl hydrogenated polycarbosilane.
A preparation method of a high-strength heat-resistant flame-retardant heat-insulating material comprises the following steps:
(1) preparing raw materials according to the weight percentage; (2) synthesizing a polyesteramide prepolymer, mixing half of total amount of ketonic anhydride and half of total amount of methanol, stirring at 50 ℃ for reaction for esterification, adding 4,4' -diaminodiphenylmethane to obtain a polyesteramide prepolymer solution, and drying to obtain polyesteramide prepolymer powder; adding the residual ketonic anhydride into the residual methanol at room temperature, heating, condensing, refluxing until the solution is transparent, pouring the solution into a stainless steel container, stirring for a certain time to obtain a polyesteramide prepolymer solution, cooling to room temperature, pouring the polyesteramide prepolymer mixed solution into a reaction kettle, putting into a vacuum drying oven, vacuumizing to-0.1 MPa, keeping at 60 ℃ for 24 hours, taking out, and grinding to obtain light yellow polyesteramide prepolymer powder; (3) uniformly mixing polyesteramide prepolymer powder, polyarylethernitrile, phosphonitrile fluoride rubber, phthalonitrile, chromite powder, cordierite powder, cyanite powder, a regulator, polycarbosilane, magnesium aluminate spinel powder and lanthanum hexaboride, adding into a mold, placing the mold into a 2450MHZ microwave oven for 1min, then placing the mold into a muffle furnace at 280 ℃, introducing nitrogen as a protective gas, keeping for 30min, raising the temperature of the muffle furnace to 310 ℃, and keeping for 40 min; (4) pouring out the viscous mixture in the die, melting and plasticizing at 310-350 ℃ in a double-screw extruder, mixing a curing agent and a foaming agent during the process, taking nitrogen as protective gas, quenching to below 50 ℃, introducing supercritical carbon dioxide, carrying out saturated adsorption, wherein the saturated adsorption pressure is 50MPa, the saturated adsorption time is 30h, the saturated adsorption temperature is 25 ℃, releasing pressure from the supercritical carbon dioxide, taking out, rapidly placing in an oil bath at 350 ℃ for foaming, the foaming time is 2min, quenching in distilled water at room temperature after foaming is finished, cleaning, shaping, and carrying out vacuum drying to obtain the high-strength heat-resistant flame-retardant heat-insulating material.
Example 2
A high-strength heat-resistant flame-retardant heat-insulation material is prepared from the following raw materials in parts by weight: 23 parts of poly (arylene ether nitrile), 33 parts of ketone anhydride, 11 parts of fluorinated phosphazene rubber, 7 parts of phthalonitrile, 3 parts of chromolite powder, 2 parts of cordierite powder, 3 parts of 4,4' -diaminodiphenylmethane, 4 parts of cyanite powder, 0.5 part of curing agent, 5 parts of polycarbosilane, 3 parts of magnesium aluminate spinel powder, 1 part of lanthanum hexaboride, 1.5 parts of foaming agent and 45 parts of methanol.
Further, the fluoroether rubber is binary copolymerization fluoroether rubber, and the fluorine content of the fluoroether rubber is 24-37%.
Further, the curing agent is a mixture of bis- [ gamma- (triethoxysilyl) propyl ] tetrasulfide, dicyandiamide and sebacic dihydrazide, and the proportion of the curing agent is 2: 5.
Further, the foaming agent is trihydrazinotriazine, 4' -oxybis (benzenesulfonylamino urea) and barium azodicarboxylate.
Further, the polycarbosilane is allyl hydrogenated polycarbosilane.
A preparation method of a high-strength heat-resistant flame-retardant heat-insulating material comprises the following steps:
(1) preparing raw materials according to the weight percentage; (2) synthesizing a polyesteramide prepolymer, mixing half of total amount of ketonic anhydride and half of total amount of methanol, stirring at 50 ℃ for reaction for esterification, adding 4,4' -diaminodiphenylmethane to obtain a polyesteramide prepolymer solution, and drying to obtain polyesteramide prepolymer powder; adding the residual ketonic anhydride into the residual methanol at room temperature, heating, condensing, refluxing until the solution is transparent, pouring the solution into a stainless steel container, stirring for a certain time to obtain a polyesteramide prepolymer solution, cooling to room temperature, pouring the polyesteramide prepolymer mixed solution into a reaction kettle, putting the reaction kettle into a vacuum drying oven, vacuumizing to-0.1 MPa, keeping the temperature at 50-60 ℃ for 24 hours, taking out, and milling to obtain light yellow polyesteramide prepolymer powder; (3) uniformly mixing polyesteramide prepolymer powder, polyarylethernitrile, phosphonitrile fluoride rubber, phthalonitrile, chromite powder, cordierite powder, cyanite powder, a regulator, polycarbosilane, magnesium aluminate spinel powder and lanthanum hexaboride, adding into a mold, placing the mold into a 2450-2500 MHZ microwave oven for 1min, then placing the mold into a 280 ℃ muffle furnace, introducing nitrogen as a protective gas, keeping for 30min, raising the temperature of the muffle furnace to 310 ℃, and keeping for 20 min; (4) pouring out the viscous mixture in the die, melting and plasticizing at 340 ℃ in a double-screw extruder, mixing a curing agent and a foaming agent during the process, taking nitrogen as protective gas, quenching to below 50 ℃, introducing supercritical carbon dioxide, carrying out saturated adsorption, wherein the saturated adsorption pressure is 50MPa, the saturated adsorption time is 28h, the saturated adsorption temperature is 10 ℃, releasing pressure from the supercritical carbon dioxide, taking out, rapidly placing in an oil bath at 350 ℃ for foaming, the foaming time is 2min, quenching in distilled water at room temperature after foaming is finished, cleaning, shaping, and carrying out vacuum drying to obtain the high-strength heat-resistant flame-retardant heat-insulating material.
TABLE 1 Performance test results of the high-strength, heat-resistant, flame-retardant, and thermal insulation materials of the examples
Table 1:
note: reference GB/T2406.2 plastic uses oxygen index method to determine burning behavior part 2. test GB/T2408 plastic burning performance at room temperature, horizontal method and vertical method GB/T2918-1998 plastic sample state adjustment and test standard environment GB/T6342 foam and rubber linear dimension determination GB/T6343 foam and rubber apparent density determination.
Determination of compression set of flexible foam polymeric materials GB/T6669 method for accelerated ageing tests for flexible and rigid foam polymeric materials GB/T9640.
GB/T10295 heat-insulating material steady-state thermal resistance and correlation measurement heat flow meter method; measuring the performance of the GB/T11547 plastic in resisting liquid chemical reagents; measurement of sound absorption coefficient and sound impedance in GB/T18696.1 Acoustic impedance tube part 1 measurement of moisture absorption property of damp heat property of GB/T20312 building material and product by standing wave ratio method.

Claims (6)

1. The high-strength heat-resistant flame-retardant heat-insulation material is characterized by being prepared from the following raw materials in parts by weight: 23-45 parts of poly (arylene ether nitrile), 33-54 parts of ketone anhydride, 11-17 parts of fluorinated phosphazene rubber, 7-13 parts of phthalonitrile, 3-7 parts of chromite powder, 2-5 parts of cordierite powder, 3-6 parts of 4,4' -diaminodiphenylmethane, 4-7 parts of cyanite powder, 0.5-1 part of curing agent, 5-8 parts of polycarbosilane, 3-6 parts of magnesium aluminate spinel powder, 1-2 parts of lanthanum hexaboride, 1-1.5 parts of foaming agent and 45-68 parts of methanol.
2. The high-strength heat-resistant flame-retardant heat-insulating material as claimed in claim 1, wherein the fluoroether rubber is binary copolymer fluoroether rubber, and the content of fluorine in the binary copolymer fluoroether rubber is 24-37%.
3. The high-strength heat-resistant flame-retardant heat-insulating material as claimed in claim 1, wherein the curing agent is a mixture of bis- [ gamma- (triethoxysilyl) propyl ] tetrasulfide, dicyandiamide, and sebacic dihydrazide, and the ratio is 1-2: 2-4: 3-5.
4. A high strength heat resistant flame retardant insulation material as claimed in claim 1, wherein said blowing agent is one or more of trihydrazinotriazine, 4' -oxybis (benzenesulfonylamino urea), barium azodicarboxylate.
5. A high strength heat resistant flame retardant insulation material as claimed in claim 1, wherein said polycarbosilane is allylhydro polycarbosilane.
6. The high-strength heat-resistant flame-retardant heat-preservation material as claimed in claim 1, characterized in that the preparation method comprises the following steps:
(1) preparing raw materials according to the weight percentage; (2) synthesizing a polyesteramide prepolymer, mixing half of total amount of ketonic anhydride and half of total amount of methanol, stirring at 50 ℃ for reaction for esterification, adding 4,4' -diaminodiphenylmethane to obtain a polyesteramide prepolymer solution, and drying to obtain polyesteramide prepolymer powder; adding the residual ketonic anhydride into the residual methanol at room temperature, heating, condensing, refluxing until the solution is transparent, pouring the solution into a stainless steel container, stirring for a certain time to obtain a polyesteramide prepolymer solution, cooling to room temperature, pouring the polyesteramide prepolymer mixed solution into a reaction kettle, putting the reaction kettle into a vacuum drying oven, vacuumizing to-0.1 MPa, keeping the temperature at 50-60 ℃ for 24 hours, taking out, and milling to obtain light yellow polyesteramide prepolymer powder; (3) uniformly mixing polyesteramide prepolymer powder, poly (arylene ether nitrile), phosphonitrile fluoride rubber, phthalonitrile, chromite powder, cordierite powder, kyanite powder, polycarbosilane, magnesium aluminate spinel powder and lanthanum hexaboride, adding into a mold, placing the mold into a 2450-2500 MHZ microwave oven, keeping for 0.5-1 min, then placing the mold into a muffle furnace at 280 ℃, introducing nitrogen as a protective gas, keeping for 10-30 min, raising the temperature of the muffle furnace to 310 ℃, and keeping for 20-40 min; (4) and pouring out the viscous mixture in the die, melting and plasticizing at 310-350 ℃ in a double-screw extruder, mixing a curing agent and a foaming agent during the process, quenching to below 50 ℃ by taking nitrogen as protective gas, introducing supercritical carbon dioxide, carrying out saturated adsorption, wherein the saturated adsorption pressure is 42-50 MPa, the saturated adsorption time is 28-30 h, the saturated adsorption temperature is-5-25 ℃, releasing pressure from the supercritical carbon dioxide, taking out, rapidly placing in an oil bath at 240-350 ℃ for foaming for 1-2min, quenching in distilled water at room temperature after foaming is finished, cleaning and shaping, and carrying out vacuum drying to obtain the high-strength heat-resistant flame-retardant heat-insulating material.
CN201911181022.1A 2019-11-27 2019-11-27 High-strength heat-resistant flame-retardant heat-insulating material Pending CN110746761A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201911181022.1A CN110746761A (en) 2019-11-27 2019-11-27 High-strength heat-resistant flame-retardant heat-insulating material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201911181022.1A CN110746761A (en) 2019-11-27 2019-11-27 High-strength heat-resistant flame-retardant heat-insulating material

Publications (1)

Publication Number Publication Date
CN110746761A true CN110746761A (en) 2020-02-04

Family

ID=69284754

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201911181022.1A Pending CN110746761A (en) 2019-11-27 2019-11-27 High-strength heat-resistant flame-retardant heat-insulating material

Country Status (1)

Country Link
CN (1) CN110746761A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116496489A (en) * 2023-06-30 2023-07-28 富海(东营)新材料科技有限公司 Preparation process of multifunctional semi-aromatic nylon

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107556512A (en) * 2017-08-16 2018-01-09 宜宾天原集团股份有限公司 Utilize supercritical CO2The method for preparing micropore poly (arylene ether nitrile) resin expanded material
CN110016221A (en) * 2019-05-05 2019-07-16 蚌埠创特新材料科技有限公司 A kind of fire resistant anticorrosive inlet manifold sealing ring material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107556512A (en) * 2017-08-16 2018-01-09 宜宾天原集团股份有限公司 Utilize supercritical CO2The method for preparing micropore poly (arylene ether nitrile) resin expanded material
CN110016221A (en) * 2019-05-05 2019-07-16 蚌埠创特新材料科技有限公司 A kind of fire resistant anticorrosive inlet manifold sealing ring material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
齐娜等: ""聚酰亚胺泡沫材料的制备与性能表征"" *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116496489A (en) * 2023-06-30 2023-07-28 富海(东营)新材料科技有限公司 Preparation process of multifunctional semi-aromatic nylon
CN116496489B (en) * 2023-06-30 2023-09-05 富海(东营)新材料科技有限公司 Preparation process of multifunctional semi-aromatic nylon

Similar Documents

Publication Publication Date Title
CN105111676B (en) A kind of preparation method and applications of the light strong plate of phenolic foam composite material
CN109504090B (en) Cold-flow-inhibiting flame-retardant impact-hardening gel and preparation method and application thereof
CN110746761A (en) High-strength heat-resistant flame-retardant heat-insulating material
CN103421270A (en) ABS material and preparation method thereof
CN106700525A (en) High-impact halogen-free flame-retardant POK/PA (polyketone/polyamide) alloy material
CN101029164B (en) Urea-resin foaming thermal-insulating composite powder, the synthetic board therewith and method
CN106867360A (en) A kind of radiator graphene powder coating and its preparation technology
CN104611941B (en) A kind of fire-retardant emulational leather material of polyvinyl chloride
CN109666228B (en) Graphene polystyrene board and preparation method thereof
CN110746575A (en) Preparation method of environment-friendly high-temperature-resistant epoxy impregnating resin
CN106243692A (en) The polyurethane resin insulation material of high-hydroscopicity
CN107418136A (en) A kind of composite foam insulation material and preparation method thereof
CN103467852B (en) A kind of Polypropylene flame-retardant plastic
CN112430013A (en) High-molecular two-component high-temperature-resistant heat-insulating material and application thereof
CN102850569B (en) Preparation method of polyimide foam
CN109867942B (en) Preparation method of flame-retardant micro-foaming polyphenyl ether composite material and product thereof
CN114989756B (en) High-temperature-resistant flame-retardant epoxy adhesive and preparation method thereof
CN104693632B (en) A kind of non-ignitable external wall insulation of A levels
CN110964329A (en) Hollow glass bead composite phthalonitrile resin rigid foam and preparation method thereof
CN107501856B (en) Preparation method of flame-retardant modified wood fiber composite phenolic foam
CN112745677B (en) High-toughness polyimide sound-absorbing foam material and preparation method thereof
CN111378245B (en) Bendable epoxy resin fireproof plate and preparation method thereof
CN113061335A (en) Environment-friendly flame-retardant building heat-insulating material and preparation method thereof
KR20140147892A (en) Highly polymeric fiber of boron carbide
CN108794968B (en) High-strength flame-retardant ABS (acrylonitrile-butadiene-styrene) alloy 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
RJ01 Rejection of invention patent application after publication

Application publication date: 20200204

RJ01 Rejection of invention patent application after publication