CN111732844A - Household fireproof coating and preparation method thereof - Google Patents

Household fireproof coating and preparation method thereof Download PDF

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Publication number
CN111732844A
CN111732844A CN202010652060.7A CN202010652060A CN111732844A CN 111732844 A CN111732844 A CN 111732844A CN 202010652060 A CN202010652060 A CN 202010652060A CN 111732844 A CN111732844 A CN 111732844A
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parts
allyl
fireproof coating
polyethylene glycol
household
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高雪梅
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D4/00Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
    • C09D4/06Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09D159/00 - C09D187/00
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18Fireproof paints including high temperature resistant paints
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/65Additives macromolecular
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/70Additives characterised by shape, e.g. fibres, flakes or microspheres

Abstract

The invention discloses a household fireproof coating which is characterized by being prepared from the following raw materials in parts by weight: 3-5 parts of hyperbranched star-shaped polyionic liquid, 1-3 parts of 2-aza-1, N6-vinyl adenosine-3 ',5' -cyclic monophosphate sodium salt, 1-3 parts of N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine/1- (9-H-fluorene-9-methyl) piperazine-1, 2, 4-tricarboxylic acid-4-allyl ester/(1-allyl-1H-benzimidazole-2-yl) methanol/diphenyl p-vinyl phosphine/polyethylene glycol monoallyl ether copolymer, 8-16 parts of inorganic filler, 12-18 parts of solvent, 1-3 parts of defoaming agent, 1-3 parts of polyethylene glycol monoallyl ether copolymer, and the like, And 1-2 parts of a leveling agent. The invention also discloses a preparation method of the household fireproof coating. The household fireproof coating disclosed by the invention has the advantages of obvious fireproof effect, good performance stability, weather resistance and environmental protection, large bonding strength with a base material, good comprehensive performance and freezing resistance, safety in use, environmental protection and long service life, and effectively realizes multiplication of economic benefit, social benefit and ecological benefit.

Description

Household fireproof coating and preparation method thereof
Technical Field
The invention relates to the technical field of coatings, in particular to a household fireproof coating and a preparation method thereof.
Background
In recent years, with the progress of global industrialization, environmental problems and energy problems are still increasingly severe, people have deeper and deeper knowledge on improving the living environment of homes and improving the physical quality of the people, have higher and higher requirements on the safety and comfort of the home life, and have more and more requirements on the functional requirements and the environmental performance of decorative materials. On the basis of the existing decoration materials, researchers in the industry need to solve the problem of endowing the decoration materials with more functions and improving the value added value of the decoration materials.
The coating is a common home decoration material, is coated on the surface of a protected or decorated object, and can form a firmly attached continuous film with the coated object. Generally, the coating is a viscous liquid prepared by using resin (or oil or emulsion) as a main material, adding corresponding auxiliary agents, adding or not adding pigments and fillers and using an organic solvent or water. At present, in home decoration, the aspects of beauty, comfort and the like are concerned, and the properties of residents are closely related, and in the existing building decoration industry, special paint is smeared on the surface of a wall body of a house, so that the performance of the wall body is greatly improved through the effect of the paint.
In the household environment, various flammable materials are more and more commonly used, and the fire prevention work is very important. One of the most common fire-retardant treatments is the use of fire-retardant coatings. The fireproof paint is a special paint used for coating the surface of a substrate, reducing the flammability of the surface of a coated material, retarding the rapid spread of fire and improving the fire endurance of the coated material. The fireproof coating has a good protective effect on a base material, and is suitable for places with visible open fire such as kitchens and the like and places with flammable plates such as wood cabinets, floors and the like. In case of fire, the fire-retardant coating which is difficult to burn in case of fire can gain time for fire extinguishing and personnel evacuation. However, the fireproof coating in the prior art has the defects of complex formula, high cost, poor fireproof performance of some products, easy cracking and influence on use. China is wide, the climate and temperature difference between east, west, south and north is large, some fireproof coatings are suitable for south, some fireproof coatings are suitable for north, most fireproof coatings have poor frost resistance, and the functions are incomplete. In addition, the fireproof coating on the market has the defects of poor performance stability, weak weather resistance and poor environmental protection performance.
The invention discloses a Chinese patent with application number 201610978339.8, which relates to a household fireproof paint, comprising the following main components: epoxy resin, polyester resin, an epoxy curing agent, a flatting agent, titanium dioxide, pentaerythritol, 5-phenyl tetrazole and the balance of filler and auxiliary agent. The household fireproof coating has the advantages of long fireproof time, high expansion rate and good heat insulation performance, and the 5-phenyltetrazole absorbs heat during decomposition and releases inert gas nitrogen, so that the household fireproof coating has good application value in fireproof coatings; however, such coatings are to be further improved in weatherability and performance stability.
Disclosure of Invention
The invention mainly aims to provide the household fireproof coating and the preparation method thereof, and the preparation method has the advantages of simple process, convenient operation and control, high production efficiency and yield and suitability for large-scale production; the household fireproof coating prepared by the preparation method has the advantages of obvious fireproof effect, good performance stability, weather resistance and environmental protection, high bonding strength with a base material, good comprehensive performance and freezing resistance, safety in use, environmental protection and long service life, and effectively realizes multiplication of economic benefit, social benefit and ecological benefit.
In order to achieve the above purposes, the technical scheme adopted by the invention is as follows:
the household fireproof coating is characterized by being prepared from the following raw materials in parts by weight: 3-5 parts of hyperbranched star-shaped polyionic liquid, 1-3 parts of 2-aza-1, N6-vinyl adenosine-3 ',5' -cyclic monophosphate sodium salt, 1-3 parts of N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine/1- (9-H-fluorene-9-methyl) piperazine-1, 2, 4-tricarboxylic acid-4-allyl ester/(1-allyl-1H-benzimidazole-2-yl) methanol/diphenyl p-vinyl phosphine/polyethylene glycol monoallyl ether copolymer, 8-16 parts of inorganic filler, 12-18 parts of solvent, 1-3 parts of defoaming agent, 1-3 parts of polyethylene glycol monoallyl ether copolymer, and the like, And 1-2 parts of a leveling agent.
Preferably, the preparation method of the hyperbranched star-shaped polyion liquid is described in chinese patent application No. CN201711143183.2, example 1.
Preferably, the leveling agent is selected from one or two of acrylate and polydimethylsiloxane; the antifoaming agent is one or more of tributyl phosphate, antifoaming agent Demodex 3100 and antifoaming agent BYK 088.
Preferably, the solvent is at least one of cyclohexanone, acetone, glycerol and butanol.
Preferably, the inorganic filler is at least one of attapulgite, medical stone and basalt fiber powder.
Preferably, the preparation method of the N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine/1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester/(1-allyl-1H-benzimidazole-2-yl) methanol/diphenyl p-styryl phosphine/polyethylene glycol monoallyl ether copolymer comprises the following steps: uniformly mixing N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine, 1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester, (1-allyl-1H-benzimidazole-2-yl) methanol, diphenyl p-styryl phosphine, polyethylene glycol monoallyl ether, a photoinitiator and a high boiling point solvent, placing the mixture in an inert gas atmosphere, irradiating the mixture for 30 to 50 minutes under ultraviolet light with the wavelength of 200 and 260nm, precipitating the mixture in water, and performing rotary evaporation to remove water to obtain the N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine/1- (9-H-fluorene-9-methyl) hydrogen Piperazine-1, 2, 4-tricarboxylic acid-4-allyl ester/(1-allyl-1H-benzimidazol-2-yl) methanol/diphenyl-p-styrylphosphine/polyethylene glycol monoallyl ether copolymer.
Preferably, the mass ratio of the N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine to the 1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester to the (1-allyl-1H-benzimidazol-2-yl) methanol to the diphenyl-p-styryl phosphine to the polyethylene glycol monoallyl ether to the photoinitiator to the high boiling point solvent is 1:2:1:0.3:1 (0.05-0.06): 20-30.
Preferably, the photoinitiator is at least one of benzoin, benzoin ethyl ether and benzoin isopropyl ether.
Preferably, the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone.
Preferably, the inert gas is any one of helium, neon and argon.
The invention also aims to provide a preparation method of the household fireproof coating, which is characterized by comprising the following steps: mixing the raw materials except the solvent according to the parts by weight, grinding the mixture through a 800-sand 1300-mesh sieve, adding the solvent, mixing uniformly, continuing to grind the mixture to the fineness of 4-12 mu m, and standing for 1-2 hours to obtain the finished product of the household fireproof coating.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
(1) according to the preparation method of the household fireproof coating, the components are directly mixed and uniformly ground to the required fineness without a special emulsification process or equipment, the preparation method is simple in process, convenient to operate and control, high in production efficiency and yield, low in production cost, easy in obtaining of production raw materials, suitable for large-scale production and high in popularization and application value.
(2) The household fireproof coating is prepared from the following raw materials in parts by weight: 3-5 parts of hyperbranched star-shaped polyionic liquid, 1-3 parts of 2-aza-1, N6-vinyl adenosine-3 ',5' -cyclic monophosphate sodium salt, 1-3 parts of N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine/1- (9-H-fluorene-9-methyl) piperazine-1, 2, 4-tricarboxylic acid-4-allyl ester/(1-allyl-1H-benzimidazole-2-yl) methanol/diphenyl p-vinyl phosphine/polyethylene glycol monoallyl ether copolymer, 8-16 parts of inorganic filler, 12-18 parts of solvent, 1-3 parts of defoaming agent, 1-3 parts of polyethylene glycol monoallyl ether copolymer, and the like, And 1-2 parts of a leveling agent. The components have synergistic effect, can effectively overcome the defects of poor performance stability, weak weather resistance, poor environmental protection performance and insignificant fireproof effect of the traditional fireproof coating, has the advantages of obvious fireproof effect, good performance stability, weather resistance and environmental protection, high bonding strength with a base material, good comprehensive performance and freezing resistance, safe use, environmental protection and long service life, and can effectively realize the increment of economic benefit, social benefit and ecological benefit.
(3) According to the household fireproof coating, a cationic group on the hyperbranched star-shaped polyionic liquid is connected with a carboxylic acid group on a copolymer through ion exchange in an ion exchange manner in the coating curing and forming stage, and can also be subjected to ion exchange reaction with 2-aza-1, N6-ethylene adenosine-3 ',5' -cyclic monophosphate sodium salt, so that main components of the coating are connected through chemical bonds to form an organic whole, and the comprehensive performance and the performance stability of the coating can be effectively improved.
(4) According to the household fireproof coating, the polyion liquid structure and the multi-nitrogen and phosphine based structures on the copolymer act synergistically under the multiple actions of an electronic effect and a position effect, so that the weather resistance of the coating is improved to a great extent; the comprehensive performance is improved, and more importantly, the fireproof performance is more excellent.
(5) In the added components of the household fireproof coating, the molecular chain of the organic component contains more active groups such as ionic groups, hydroxyl groups, carboxyl groups, amino groups and the like, and the bonding property of the coating and a substrate can be improved through the bridging effect; the copolymer is used as a film forming substance, and the nitrogen-1, N6-ethylene adenosine, phenyl [1,2,4] triazolo [3,4-a ] phthalazine, benzimidazole alcohol and phenylphosphine structures introduced into the molecular chain of the copolymer synergistically act to improve the comprehensive performance of the coating, so that the service life of the fireproof coating is prolonged, and the fireproof coating contains less halogen such as chloride ions and the like, and has good environmental protection performance.
Detailed Description
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art.
The raw materials in the embodiment of the invention are all purchased commercially; the preparation method of the hyperbranched star-shaped polyion liquid is disclosed in the patent example 1 of the Chinese invention with the application number of CN 201711143183.2.
Example 1
The household fireproof coating is characterized by being prepared from the following raw materials in parts by weight: 3 parts of hyperbranched star-shaped polyion liquid, 1 part of 2-aza-1, N6-vinyl adenosine-3 ',5' -cyclic monophosphate sodium salt, 45 parts of N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine/1- (9-H-fluorene-9-methyl) piperazine-1, 2, 4-tricarboxylic acid-4-allyl ester/(1-allyl-1H-benzimidazole-2-yl) methanol/diphenyl p-phenyl vinyl phosphine/polyethylene glycol monoallyl ether copolymer, 8 parts of inorganic filler, 12 parts of solvent, 1 part of defoaming agent and 1 part of leveling agent.
The leveling agent is selected from acrylic ester; the defoaming agent is tributyl phosphate; the solvent is cyclohexanone;
the inorganic filler is attapulgite.
The preparation method of the N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine/1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester/(1-allyl-1H-benzimidazole-2-yl) methanol/diphenyl-p-styrylphosphine/polyethylene glycol monoallyl ether copolymer comprises the following steps: uniformly mixing N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine, 1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester, (1-allyl-1H-benzimidazole-2-yl) methanol, diphenyl p-styryl phosphine, polyethylene glycol monoallyl ether, a photoinitiator and a high boiling point solvent, placing the mixture in an inert gas atmosphere, irradiating the mixture for 30 minutes under ultraviolet light with the wavelength of 200nm, precipitating the mixture in water, and performing rotary evaporation to remove water to obtain the N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine/1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester/(1-allyl-1H-benzimidazol-2-yl) methanol/diphenyl p-styrylphosphine/polyethylene glycol monoallyl ether copolymer.
The mass ratio of the N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine to the 1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester to the (1-allyl-1H-benzimidazole-2-yl) methanol to the diphenyl-p-styryl phosphine to the polyethylene glycol monoallyl ether to the photoinitiator to the high-boiling point solvent is 1:2:1:0.3:1:0.05: 20; the photoinitiator is benzoin; the high boiling point solvent is dimethyl sulfoxide; the inert gas is helium.
The preparation method of the household fireproof coating is characterized by comprising the following steps: mixing the raw materials except the solvent according to parts by weight, grinding and sieving through a 800-mesh sieve, adding the solvent, mixing uniformly, continuously grinding to the fineness of 4 mu m, and standing for 1 hour to obtain the finished product of the household fireproof coating.
Example 2
The household fireproof coating is characterized by being prepared from the following raw materials in parts by weight: 3.5 parts of hyperbranched star-shaped polyion liquid, 1.5 parts of 2-aza-1, N6-vinyl adenosine-3 ',5' -cyclic monophosphate sodium salt, 1.5 parts of N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine/1- (9-H-fluorene-9-methyl) piperazine-1, 2, 4-tricarboxylic acid-4-allyl ester/(1-allyl-1H-benzimidazole-2-yl) methanol/diphenyl p-styryl phosphine/polyethylene glycol monoallyl ether copolymer, 9 parts of inorganic filler, 13 parts of solvent, 1.5 parts of defoaming agent and 1.2 parts of flatting agent.
The leveling agent is selected from polydimethylsiloxane; the antifoaming agent is antifoaming agent delete 3100; the solvent is acetone; the inorganic filler is medical stone.
The preparation method of the N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine/1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester/(1-allyl-1H-benzimidazole-2-yl) methanol/diphenyl-p-styrylphosphine/polyethylene glycol monoallyl ether copolymer comprises the following steps: uniformly mixing N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine, 1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester, (1-allyl-1H-benzimidazole-2-yl) methanol, diphenyl p-styryl phosphine, polyethylene glycol monoallyl ether, a photoinitiator and a high boiling point solvent, placing the mixture in an inert gas atmosphere, irradiating the mixture for 35 minutes under ultraviolet light with the wavelength of 220nm, precipitating the mixture in water, and performing rotary evaporation to remove water to obtain the N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine/1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester/(1-allyl-1H-benzimidazol-2-yl) methanol/diphenyl p-styrylphosphine/polyethylene glycol monoallyl ether copolymer.
The mass ratio of the N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine to the 1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester to the (1-allyl-1H-benzimidazole-2-yl) methanol to the diphenyl-p-styryl phosphine to the polyethylene glycol monoallyl ether to the photoinitiator to the high-boiling point solvent is 1:2:1:0.3:1:0.052: 23; the photoinitiator is benzoin ethyl ether; the high boiling point solvent is N, N-dimethylformamide; the inert gas is neon.
The preparation method of the household fireproof coating is characterized by comprising the following steps: mixing the raw materials except the solvent according to parts by weight, grinding the mixture and sieving the mixture by a 900-mesh sieve, adding the solvent, mixing the mixture evenly, continuously grinding the mixture to the fineness of 6 mu m, and standing the mixture for 1.2 hours to obtain the finished product of the household fireproof coating.
Example 3
The household fireproof coating is characterized by being prepared from the following raw materials in parts by weight: 4 parts of hyperbranched star-shaped polyion liquid, 2-aza-1, N6-vinyl adenosine-3 ',5' -cyclic monophosphate sodium salt, 2 parts of N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine/1- (9-H-fluorene-9-methyl) piperazine-1, 2, 4-tricarboxylic acid-4-allyl ester/(1-allyl-1H-benzimidazole-2-yl) methanol/diphenyl p-phenyl vinyl phosphine/polyethylene glycol monoallyl ether copolymer, 13 parts of inorganic filler, 15 parts of solvent, 2 parts of defoaming agent and 1.5 parts of leveling agent.
The leveling agent is selected from acrylic ester; the defoaming agent is a defoaming agent BYK 088; the solvent is glycerol; the inorganic filler is basalt fiber powder.
The preparation method of the N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine/1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester/(1-allyl-1H-benzimidazole-2-yl) methanol/diphenyl-p-styrylphosphine/polyethylene glycol monoallyl ether copolymer comprises the following steps: uniformly mixing N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine, 1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester, (1-allyl-1H-benzimidazole-2-yl) methanol, diphenyl p-styryl phosphine, polyethylene glycol monoallyl ether, a photoinitiator and a high boiling point solvent, placing the mixture in an inert gas atmosphere, irradiating the mixture for 40 minutes under the ultraviolet light with the wavelength of 235nm, precipitating the mixture in water, and performing rotary evaporation to remove water to obtain the N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine/1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester/(1-allyl-1H-benzimidazol-2-yl) methanol/diphenyl p-styrylphosphine/polyethylene glycol monoallyl ether copolymer.
The mass ratio of the N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine to the 1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester to the (1-allyl-1H-benzimidazole-2-yl) methanol to the diphenyl-p-styryl phosphine to the polyethylene glycol monoallyl ether to the photoinitiator to the high-boiling-point solvent is 1:2:1:0.3:1:0.055: 25.
The photoinitiator is benzoin isopropyl ether; the high boiling point solvent is N, N-dimethylacetamide; the inert gas is argon.
The preparation method of the household fireproof coating is characterized by comprising the following steps: mixing the raw materials except the solvent according to parts by weight, grinding and sieving through a 1100-mesh sieve, adding the solvent, mixing uniformly, continuously grinding to the fineness of 9 mu m, and standing for 1.5 hours to obtain the finished product of the household fireproof coating.
Example 4
The household fireproof coating is characterized by being prepared from the following raw materials in parts by weight: 4.5 parts of hyperbranched star-shaped polyionic liquid, 2-aza-1, N6-vinyl adenosine-3 ',5' -cyclic monophosphate sodium salt 2.5 parts, N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine/1- (9-H-fluorene-9-methyl) piperazine-1, 2, 4-tricarboxylic acid-4-allyl ester/(1-allyl-1H-benzimidazole-2-yl) methanol/diphenyl p-styryl phosphine/polyethylene glycol monoallyl ether copolymer 53 parts, 14 parts of inorganic filler, 17 parts of solvent, 2.5 parts of defoaming agent and 1.9 parts of flatting agent.
The leveling agent is formed by mixing acrylic ester and polydimethylsiloxane in a mass ratio of 2: 1; the defoaming agent is formed by mixing tributyl phosphate, a defoaming agent Demodex 3100 and a defoaming agent BYK088 according to the mass ratio of 1:1: 2; the solvent is formed by mixing cyclohexanone, acetone, glycerol and butanol according to the mass ratio of 1:1:3: 2; the inorganic filler is formed by mixing attapulgite, medical stone and basalt fiber powder according to the mass ratio of 2:4: 7.
The preparation method of the N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine/1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester/(1-allyl-1H-benzimidazole-2-yl) methanol/diphenyl-p-styrylphosphine/polyethylene glycol monoallyl ether copolymer comprises the following steps: uniformly mixing N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine, 1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester, (1-allyl-1H-benzimidazole-2-yl) methanol, diphenyl p-styryl phosphine, polyethylene glycol monoallyl ether, a photoinitiator and a high boiling point solvent, placing the mixture in an inert gas atmosphere, irradiating the mixture for 45 minutes under ultraviolet light with the wavelength of 250nm, precipitating the mixture in water, and performing rotary evaporation to remove water to obtain the N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine/1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester/(1-allyl-1H-benzimidazol-2-yl) methanol/diphenyl p-styrylphosphine/polyethylene glycol monoallyl ether copolymer.
The mass ratio of the N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine to the 1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester to the (1-allyl-1H-benzimidazole-2-yl) methanol to the diphenyl-p-styryl phosphine to the polyethylene glycol monoallyl ether to the photoinitiator to the high-boiling point solvent is 1:2:1:0.3:1:0.059: 28; the photoinitiator is formed by mixing benzoin, benzoin ethyl ether and benzoin isopropyl ether according to the mass ratio of 1:3: 2; the high-boiling-point solvent is formed by mixing dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone according to a mass ratio of 1:3:5: 3; the inert gas is helium.
The preparation method of the household fireproof coating is characterized by comprising the following steps: mixing the raw materials except the solvent in parts by weight, grinding the mixture and sieving the mixture through a 1200-mesh sieve, adding the solvent, mixing the mixture evenly, continuing to grind the mixture to the fineness of 11 mu m, and standing the mixture for 1.8 hours to obtain the finished product of the household fireproof coating.
Example 5
The household fireproof coating is characterized by being prepared from the following raw materials in parts by weight: 5 parts of hyperbranched star-shaped polyion liquid, 3 parts of 2-aza-1, N6-vinyl adenosine-3 ',5' -cyclic monophosphate sodium salt, 55 parts of N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine/1- (9-H-fluorene-9-methyl) piperazine-1, 2, 4-tricarboxylic acid-4-allyl ester/(1-allyl-1H-benzimidazole-2-yl) methanol/diphenyl p-phenyl vinyl phosphine/polyethylene glycol monoallyl ether copolymer, 16 parts of inorganic filler, 18 parts of solvent, 3 parts of defoaming agent and 2 parts of leveling agent.
The leveling agent is selected from acrylic ester; the defoaming agent is tributyl phosphate; the solvent is butanol; the inorganic filler is basalt fiber powder.
The preparation method of the N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine/1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester/(1-allyl-1H-benzimidazole-2-yl) methanol/diphenyl-p-styrylphosphine/polyethylene glycol monoallyl ether copolymer comprises the following steps: uniformly mixing N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine, 1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester, (1-allyl-1H-benzimidazole-2-yl) methanol, diphenyl p-styryl phosphine, polyethylene glycol monoallyl ether, a photoinitiator and a high boiling point solvent, placing the mixture in an inert gas atmosphere, irradiating the mixture for 50 minutes under ultraviolet light with the wavelength of 260nm, precipitating the mixture in water, and performing rotary evaporation to remove water to obtain the N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine/1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester/(1-allyl-1H-benzimidazol-2-yl) methanol/diphenyl p-styrylphosphine/polyethylene glycol monoallyl ether copolymer.
The mass ratio of the N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine to the 1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester to the (1-allyl-1H-benzimidazole-2-yl) methanol to the diphenyl-p-styryl phosphine to the polyethylene glycol monoallyl ether to the photoinitiator to the high-boiling point solvent is 1:2:1:0.3:1:0.06: 30; the photoinitiator is benzoin ethyl ether; the high boiling point solvent is N-methyl pyrrolidone; the inert gas is helium.
The preparation method of the household fireproof coating is characterized by comprising the following steps: mixing the raw materials except the solvent according to the parts by weight, grinding and sieving through a 1300-mesh sieve, adding the solvent, mixing uniformly, continuously grinding to the fineness of 12 mu m, and standing for 2 hours to obtain the finished product of the household fireproof coating.
Comparative example 1
The present example provides a home fireproofing coating, which has a formulation and a preparation method substantially the same as those of example 1, except that no hyperbranched star-shaped polyion liquid is added.
Comparative example 2
This example provides a fire retardant coating for home use, which is formulated and prepared substantially as described in example 1, except that 2-aza-1, N6-ethenyl adenosine-3 ',5' -cyclic monophosphate sodium salt is not added.
Comparative example 3
This example provides a fire retardant coating for home use, which is formulated and prepared in substantially the same manner as in example 1, except that the copolymer is prepared without the addition of N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine.
Comparative example 4
This example provides a fire retardant coating for home use, which has substantially the same formulation and preparation method as in example 1, except that 1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester was not added during the preparation of the copolymer.
Comparative example 5
This example provides a fire retardant coating for home use having substantially the same formulation and preparation as in example 1, except that the copolymer was prepared without the addition of (1-allyl-1H-benzimidazol-2-yl) methanol.
Comparative example 6
This example provides a fire retardant coating for home use, which is formulated and prepared in substantially the same manner as in example 1, except that no diphenyl-p-styryl phosphine is added to the copolymer.
The home fireproofing coatings obtained in the above examples 1-5 and comparative examples 1-6 were tested, and the test results and test methods are shown in table 1.
As can be seen from Table 1, the home fireproof coating disclosed by the embodiment of the invention has the advantages that the fireproof performance is 53.2-54.1min, the adhesion is 9.1-10.2Ma, and the water resistance is not abnormal after being soaked for 30 days, while the fireproof performance of a comparative sample is 44.2-44.9min, the adhesion is 7.6-8.8Ma, and the household fireproof coating falls off after being soaked for 30 days. Therefore, the household fireproof coating disclosed by the embodiment of the invention has better fire resistance and water resistance and stronger adhesive force, these excellent properties are the result of the synergistic effect of the hyperbranched star-like polyionic liquid 2-aza-1, N6-vinyladenosine-3 ',5' -cyclic monophosphate sodium salt, N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine/1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester/(1-allyl-1H-benzimidazol-2-yl) methanol/diphenyl p-styrylphosphine/polyethylene glycol monoallyl ether copolymer.
TABLE 1
Figure BDA0002575339970000091
The foregoing is directed to embodiments of the present invention and, more particularly, to a method and apparatus for controlling a power converter in a power converter, including a power converter, a power.

Claims (10)

1. The household fireproof coating is characterized by being prepared from the following raw materials in parts by weight: 3-5 parts of hyperbranched star-shaped polyionic liquid, 1-3 parts of 2-aza-1, N6-vinyl adenosine-3 ',5' -cyclic monophosphate sodium salt, 1-3 parts of N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine/1- (9-H-fluorene-9-methyl) piperazine-1, 2, 4-tricarboxylic acid-4-allyl ester/(1-allyl-1H-benzimidazole-2-yl) methanol/diphenyl p-vinyl phosphine/polyethylene glycol monoallyl ether copolymer, 8-16 parts of inorganic filler, 12-18 parts of solvent, 1-3 parts of defoaming agent, 1-3 parts of polyethylene glycol monoallyl ether copolymer, and the like, And 1-2 parts of a leveling agent.
2. The household fireproof coating according to claim 1, wherein the leveling agent is one or two selected from acrylate and polydimethylsiloxane; the antifoaming agent is one or more of tributyl phosphate, antifoaming agent Demodex 3100 and antifoaming agent BYK 088.
3. The household fireproof paint according to claim 1, wherein the solvent is at least one of cyclohexanone, acetone, glycerol and butanol.
4. The household fireproof coating according to claim 1, wherein the inorganic filler is at least one of attapulgite, medical stone and basalt fiber powder.
5. The household fireproof paint of claim 1, wherein the preparation method of the N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine/1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester/(1-allyl-1H-benzimidazole-2-yl) methanol/diphenyl p-styryl phosphine/polyethylene glycol monoallyl ether copolymer comprises the following steps: uniformly mixing N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine, 1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester, (1-allyl-1H-benzimidazole-2-yl) methanol, diphenyl p-styryl phosphine, polyethylene glycol monoallyl ether, a photoinitiator and a high boiling point solvent, placing the mixture in an inert gas atmosphere, irradiating the mixture for 30 to 50 minutes under ultraviolet light with the wavelength of 200 and 260nm, precipitating the mixture in water, and performing rotary evaporation to remove water to obtain the N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine/1- (9-H-fluorene-9-methyl) hydrogen Piperazine-1, 2, 4-tricarboxylic acid-4-allyl ester/(1-allyl-1H-benzimidazol-2-yl) methanol/diphenyl-p-styrylphosphine/polyethylene glycol monoallyl ether copolymer.
6. The household fireproof coating as claimed in claim 5, wherein the mass ratio of N-allyl-6-phenyl [1,2,4] triazolo [3,4-a ] phthalazin-3-amine, 1- (9-H-fluorene-9-methyl) hydropiperazine-1, 2, 4-tricarboxylic acid-4-allyl ester, (1-allyl-1H-benzimidazol-2-yl) methanol, diphenyl p-styryl phosphine, polyethylene glycol monoallyl ether, photoinitiator and high boiling point solvent is 1:2:1:0.3:1 (0.05-0.06): 20-30.
7. The household fireproof paint of claim 5, wherein the photoinitiator is at least one of benzoin, benzoin ethyl ether and benzoin isopropyl ether.
8. The household fireproof paint according to claim 5, wherein the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone.
9. The household fireproof coating of claim 1, wherein the inert gas is any one of helium, neon and argon.
10. The household fireproof coating according to any one of claims 1 to 9, wherein the preparation method of the household fireproof coating comprises the following steps: mixing the raw materials except the solvent according to the parts by weight, grinding the mixture through a 800-sand 1300-mesh sieve, adding the solvent, mixing uniformly, continuing to grind the mixture to the fineness of 4-12 mu m, and standing for 1-2 hours to obtain the finished product of the household fireproof coating.
CN202010652060.7A 2020-07-08 2020-07-08 Household fireproof coating and preparation method thereof Pending CN111732844A (en)

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