CN114213891A - Preparation method of hybrid flame retardant and water-based steel structure fireproof coating - Google Patents
Preparation method of hybrid flame retardant and water-based steel structure fireproof coating Download PDFInfo
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- CN114213891A CN114213891A CN202111497496.4A CN202111497496A CN114213891A CN 114213891 A CN114213891 A CN 114213891A CN 202111497496 A CN202111497496 A CN 202111497496A CN 114213891 A CN114213891 A CN 114213891A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING 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
- C09D201/00—Coating compositions based on unspecified macromolecular compounds
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- 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
Abstract
The invention discloses a preparation method of a hybrid flame retardant, which comprises the following steps: s1: firstly, preparing phosphorus-nitrogen-containing silane M; s2: adding M and tetraethyl orthosilicate B into a reactor according to a certain mass ratio, and dissolving in a solvent to obtain a reaction solution; s3: and (3) introducing a precipitator into the reaction solution of S2, filtering to obtain a solid-phase product, and drying the product at 50-140 ℃ to finally obtain the phosphorus-nitrogen-silicon-containing organic-inorganic hybrid flame retardant. The novel organic-inorganic hybrid halogen-free flame retardant integrating phosphorus, nitrogen and silicon is prepared by a sol-gel method reaction, has high flame retardant efficiency, and can promote carbon formation during combustion to form a compact silicon-carbon layer; the invention also discloses the water-based steel structure fireproof coating, which is prepared by adding the hybrid flame retardant, has the advantages of excellent fire resistance, water resistance and cold and heat cycle resistance, and has good fire resistance, water resistance and cold and heat cycle resistance.
Description
Technical Field
The invention relates to the technical field related to flame retardants, in particular to a preparation method of a hybrid flame retardant and a water-based steel structure fireproof coating.
Background
The flame retardant is a substance that increases the flame resistance of combustibles, and is classified into an additive type flame retardant and a reactive type flame retardant according to the method of use. Further, the halogen-based flame retardant and the halogen-free flame retardant can be classified according to whether or not the halogen-based element is contained. The halogen flame retardant eliminates active free radicals generated by combustion reaction of high polymer materials mainly through hydrogen halide generated during thermal degradation, has the advantages of high cost performance, small using amount, high flame retardant efficiency and the like, but generates a large amount of dense smoke during combustion, and simultaneously, the hydrogen halide has strong toxicity and is widely forbidden. At present, the research direction of the flame retardant is mainly halogen-free flame retardant, a phosphorus-nitrogen flame retardant system belongs to the most common flame retardant system, and polyphosphoric acid is generated by the phosphorus-containing flame retardant at high temperature, so that the carbonization of the organic base material is realized. Meanwhile, the nitrogen-containing flame retardant is decomposed when being heated, and has flame retardant effects of heat absorption, temperature reduction, dilution and the like.
Phosphorus-silicon flame retardant systems have been a relatively effective flame retardant system in recent years. The silicon-containing flame retardant can not release toxic gas in the combustion process, and meanwhile, in the thermal degradation process, the silicon-containing flame retardant is easy to migrate to the surface of the base material due to low surface energy, so that a silicon-carbon protective layer which is not easy to degrade is generated. The silicon-carbon protective layer has good thermal stability and excellent mechanical property, and can effectively prevent the further degradation of the inner-layer base material. However, these two flame retardants generally have the following disadvantages: low flame-retardant efficiency and can not solve the problem of molten drop in the combustion process of the polymer.
Disclosure of Invention
The invention aims to provide a preparation method of a hybrid flame retardant and a water-based steel structure fireproof coating, so as to solve the problems in the background technology.
In order to realize the purpose, the invention provides the following technical scheme, and the preparation method of the hybrid flame retardant comprises the following steps:
s1: the preparation of the phosphorus-nitrogen-containing silane M was carried out first, according to 1: dissolving siloxane containing imino and aldehyde compounds in a solvent according to a proportion of 1-3, heating to 30-40 ℃, and reacting for 2-5 h; then, adding dimethyl phosphite or diethyl phosphite with the same amount of substances as the aldehyde compound into a reaction system by using an automatic dropping device, then heating to 60-75 ℃, keeping for 8-20 h, and finally performing rotary evaporation purification on the product to obtain phosphorus-containing silane M with the end group of siloxane;
s2: adding M and tetraethyl orthosilicate B into a reactor according to a certain mass ratio, dissolving in a solvent at the reaction temperature of-20-150 ℃, dropwise adding deionized water, and performing condensation reaction between reactants for 1-72 hours to obtain a reaction solution;
s3: and (3) introducing a precipitator into the reaction solution of S2, filtering to obtain a solid-phase product, and drying the product at 50-140 ℃ to finally obtain the phosphorus-nitrogen-silicon-containing organic-inorganic hybrid flame retardant.
The water-based steel structure fireproof coating is prepared by adding a hybrid flame retardant, and comprises the following components in percentage by weight: 20-50% of emulsion polymer, 20-40% of hybrid flame retardant, 2-6% of film forming additive, 0.1-0.5% of wetting agent, 0.1-0.2% of flatting agent, 0.1-0.4% of thickening agent, 0.1-0.3% of defoaming agent, 0.1-0.3% of bactericide, 0.1-0.5% of ammonia water, 0.2-0.6% of preservative, 0.05-0.3% of antifreezing agent, 0.2-0.4% of anti-settling agent, 0.2-0.4% of fluorescent whitening agent and the balance of deionized water.
Preferably, the emulsion polymer adopts an anionic aliphatic polyether polyurethane dispersoid, the wetting agent is a polyacrylic acid ammonium salt or a polyacrylic acid sodium salt wetting dispersant, and the defoaming agent is a mineral oil or organosilicon defoaming agent.
Preferably, the preservative adopts a mixture of 5-chloro-2-methyl-4-isothiazolin-3-one and 2-methyl-4-isothiazolin-3-one in any proportion.
Preferably, the antifreezing agent is glycerol ethoxylate antifreezing agent, and the thickener is associative polyurethane thickener.
Preferably, the anti-settling agent is any one of organic bentonite, fumed silica, titanate coupling agent or polyamide wax.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, firstly, silane M with high phosphorus and nitrogen content is synthesized, and the characteristic that siloxane on the structure of M is easy to undergo hydrolytic condensation reaction under a catalyst is utilized, and M and tetraethyl orthosilicate are reacted by a sol-gel method to prepare the novel organic-inorganic hybrid halogen-free flame retardant integrating phosphorus, nitrogen and silicon, compared with the existing flame retardant, the reaction steps of the flame retardant are simple and easy to realize, the advantages of phosphorus-silicon and phosphorus-nitrogen systems are combined, the flame retardant has high flame retardant efficiency, and the flame retardant can promote carbon formation during combustion to form a compact silicon-carbon layer, so that secondary combustion caused by melting and dropping of a high polymer material during combustion is prevented; high flame-retardant efficiency can be formed during combustion, and no halogen is contained, so that the environment is not polluted;
2. the water-based steel structure fireproof coating prepared by the hybrid flame retardant is superior in fire resistance, water resistance and cold and heat cycle resistance, and has good fire resistance, water resistance and cold and heat cycle resistance.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a technical scheme that: the technical solution of the present patent will be described in further detail with reference to the following embodiments.
A method for preparing a hybrid flame retardant, comprising the steps of:
s1: the preparation of the phosphorus-nitrogen-containing silane M was carried out first, according to 1: dissolving siloxane containing imino and aldehyde compounds in a solvent according to a proportion of 1-3, heating to 30-40 ℃, and reacting for 2-5 h; then, adding dimethyl phosphite or diethyl phosphite with the same amount of substances as the aldehyde compound into a reaction system by using an automatic dropping device, then heating to 60-75 ℃, keeping for 8-20 h, and finally performing rotary evaporation purification on the product to obtain phosphorus-containing silane M with the end group of siloxane;
s2: adding M and tetraethyl orthosilicate B into a reactor according to a certain mass ratio, dissolving in a solvent at the reaction temperature of-20-150 ℃, dropwise adding deionized water, and performing condensation reaction between reactants for 1-72 hours to obtain a reaction solution;
s3: and (3) introducing a precipitator into the reaction solution of S2, filtering to obtain a solid-phase product, and drying the product at 50-140 ℃ to finally obtain the phosphorus-nitrogen-silicon-containing organic-inorganic hybrid flame retardant.
The water-based steel structure fireproof coating is prepared by adding a hybrid flame retardant, and comprises the following components in percentage by weight: 20-50% of emulsion polymer, 20-40% of hybrid flame retardant, 2-6% of film forming additive, 0.1-0.5% of wetting agent, 0.1-0.2% of flatting agent, 0.1-0.4% of thickening agent, 0.1-0.3% of defoaming agent, 0.1-0.3% of bactericide, 0.1-0.5% of ammonia water, 0.2-0.6% of preservative, 0.05-0.3% of antifreezing agent, 0.2-0.4% of anti-settling agent, 0.2-0.4% of fluorescent whitening agent and the balance of deionized water.
Detailed description of the preferred embodiment 1
A method for preparing a hybrid flame retardant, comprising the steps of:
s1: the preparation of the phosphorus-nitrogen-containing silane M was carried out first, according to 1: 1, dissolving siloxane containing imino and aldehyde compound in a solvent, heating to 30 ℃, and reacting for 2 hours; then, adding dimethyl phosphite or diethyl phosphite with the same amount of substances as the aldehyde compound into a reaction system by using an automatic dropping device, then heating to 60 ℃, keeping for 8 hours, and finally performing rotary evaporation purification on the product to obtain phosphorus-containing silane M with the end group of siloxane;
s2: adding M and tetraethyl orthosilicate B into a reactor according to a certain mass ratio, dissolving in a solvent at the reaction temperature of-20 ℃, dropwise adding deionized water, and carrying out condensation reaction on reactants for 1h to obtain a reaction solution;
s3: and (3) introducing a precipitator into the reaction solution of S2, filtering to obtain a solid-phase product, drying the product at 50 ℃, and finally obtaining the phosphorus-nitrogen-silicon-containing organic-inorganic hybrid flame retardant.
The water-based steel structure fireproof coating is prepared by adding a hybrid flame retardant, and comprises the following components in percentage by weight: 30% of emulsion polymer, 30% of hybrid flame retardant, 3% of film-forming assistant, 0.2% of wetting agent, 0.1% of leveling agent, 0.2% of thickening agent, 0.1% of defoaming agent, 0.1% of bactericide, 0.2% of ammonia water, 0.2% of preservative, 0.05% of antifreezing agent, 0.2% of anti-settling agent, 0.2% of fluorescent whitening agent and the balance of deionized water.
Specific example 2
A method for preparing a hybrid flame retardant, comprising the steps of:
s1: the preparation of the phosphorus-nitrogen-containing silane M was carried out first, according to 1: 2, dissolving siloxane containing imino and aldehyde compound in a solvent, heating to 35 ℃, and reacting for 3 hours; then, adding dimethyl phosphite or diethyl phosphite with the same amount of substances as the aldehyde compound into a reaction system by using an automatic dropping device, then heating to 65 ℃, keeping for 15 hours, and finally performing rotary evaporation purification on the product to obtain phosphorus-containing silane M with the end group of siloxane;
s2: adding M and tetraethyl orthosilicate B into a reactor according to a certain mass ratio, dissolving in a solvent at the reaction temperature of 80 ℃, dropwise adding deionized water, and carrying out condensation reaction on reactants for 36 hours to obtain a reaction solution;
s3: and (3) introducing a precipitator into the reaction solution of S2, filtering to obtain a solid-phase product, drying the product at 100 ℃, and finally obtaining the phosphorus-nitrogen-silicon-containing organic-inorganic hybrid flame retardant.
The water-based steel structure fireproof coating is prepared by adding a hybrid flame retardant, and comprises the following components in percentage by weight: 50% of emulsion polymer, 20% of hybrid flame retardant, 5% of film-forming assistant, 0.4% of wetting agent, 0.2% of leveling agent, 0.25% of thickening agent, 0.2% of defoaming agent, 0.2% of bactericide, 0.3% of ammonia water, 0.4% of preservative, 0.2% of antifreezing agent, 0.3% of anti-settling agent, 0.3% of fluorescent whitening agent and the balance of deionized water.
Specific example 3
A method for preparing a hybrid flame retardant, comprising the steps of:
s1: the preparation of the phosphorus-nitrogen-containing silane M was carried out first, according to 1: 3, dissolving siloxane containing imino and aldehyde compound in a solvent, heating to 40 ℃, and reacting for 5 hours; then, adding dimethyl phosphite or diethyl phosphite with the same amount of substances as the aldehyde compound into a reaction system by using an automatic dropping device, then heating to 75 ℃, keeping for 20 hours, and finally performing rotary evaporation purification on the product to obtain phosphorus-containing silane M with the end group of siloxane;
s2: adding M and tetraethyl orthosilicate B into a reactor according to a certain mass ratio, dissolving in a solvent at the reaction temperature of 150 ℃, dropwise adding deionized water, and carrying out condensation reaction on reactants for 72 hours to obtain a reaction solution;
s3: and (3) introducing a precipitator into the reaction solution of S2, filtering to obtain a solid-phase product, drying the product at 140 ℃, and finally obtaining the phosphorus-nitrogen-silicon-containing organic-inorganic hybrid flame retardant.
The water-based steel structure fireproof coating is prepared by adding a hybrid flame retardant, and comprises the following components in percentage by weight: 40% of emulsion polymer, 40% of hybrid flame retardant, 5% of film-forming assistant, 0.5% of wetting agent, 0.2% of leveling agent, 0.4% of thickening agent, 0.3% of defoaming agent, 0.3% of bactericide, 0.5% of ammonia water, 0.6% of preservative, 0.3% of antifreezing agent, 0.4% of anti-settling agent, 0.4% of fluorescent whitening agent and the balance of deionized water.
The water-based steel structure fireproof coating prepared by the embodiment of the invention has reliable storage stability, can obtain good stability by a heat storage test at 50 ℃, and has the following structure shown in the following table when detected according to GB 14907-2018 'water-based steel structure fireproof coating for steel structure':
TABLE 1
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. A preparation method of a hybrid flame retardant is characterized by comprising the following steps: the method comprises the following steps:
s1: the preparation of the phosphorus-nitrogen-containing silane M was carried out first, according to 1: dissolving siloxane containing imino and aldehyde compounds in a solvent according to a proportion of 1-3, heating to 30-40 ℃, and reacting for 2-5 h; then, adding dimethyl phosphite or diethyl phosphite with the same amount of substances as the aldehyde compound into a reaction system by using an automatic dropping device, then heating to 60-75 ℃, keeping for 8-20 h, and finally performing rotary evaporation purification on the product to obtain phosphorus-containing silane M with the end group of siloxane;
s2: adding M and tetraethyl orthosilicate B into a reactor according to a certain mass ratio, dissolving in a solvent at the reaction temperature of-20-150 ℃, dropwise adding deionized water, and performing condensation reaction between reactants for 1-72 hours to obtain a reaction solution;
s3: and (3) introducing a precipitator into the reaction solution of S2, filtering to obtain a solid-phase product, and drying the product at 50-140 ℃ to finally obtain the phosphorus-nitrogen-silicon-containing organic-inorganic hybrid flame retardant.
2. An aqueous fire-retardant coating for steel structures, which is prepared by adding the hybrid fire retardant according to claim 1, and is characterized in that: the fireproof coating is composed of the following components in percentage by weight: 20-50% of emulsion polymer, 20-40% of hybrid flame retardant, 2-6% of film forming additive, 0.1-0.5% of wetting agent, 0.1-0.2% of flatting agent, 0.1-0.4% of thickening agent, 0.1-0.3% of defoaming agent, 0.1-0.3% of bactericide, 0.1-0.5% of ammonia water, 0.2-0.6% of preservative, 0.05-0.3% of antifreezing agent, 0.2-0.4% of anti-settling agent, 0.2-0.4% of fluorescent whitening agent and the balance of deionized water.
3. The water-based fire retardant coating for steel structures of claim 2, wherein: the emulsion polymer adopts anionic aliphatic polyether polyurethane dispersoid, the wetting agent is polyacrylic acid ammonium salt or sodium polyacrylate wetting dispersant, and the defoaming agent is mineral oil or organosilicon defoaming agent.
4. The water-based fire retardant coating for steel structures of claim 2, wherein: the preservative is a mixture of 5-chloro-2-methyl-4-isothiazoline-3-ketone and 2-methyl-4-isothiazoline-3-ketone in any proportion.
5. The water-based fire retardant coating for steel structures of claim 2, wherein: the antifreezing agent is glycerol ethoxylate antifreezing agent, and the thickener is associative polyurethane thickener.
6. The water-based fire retardant coating for steel structures of claim 2, wherein: the anti-settling agent is any one of organic bentonite, fumed silica, titanate coupling agent or polyamide wax.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115591138A (en) * | 2022-10-26 | 2023-01-13 | 深圳市城市公共安全技术研究院有限公司（Cn） | Fire safety rope and preparation method thereof |
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| CN115591138A (en) * | 2022-10-26 | 2023-01-13 | 深圳市城市公共安全技术研究院有限公司（Cn） | Fire safety rope and preparation method thereof |
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Application publication date: 20220322 |