CN112358818A - Fireproof adhesive and preparation method thereof - Google Patents
Fireproof adhesive and preparation method thereof Download PDFInfo
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- CN112358818A CN112358818A CN202011341297.XA CN202011341297A CN112358818A CN 112358818 A CN112358818 A CN 112358818A CN 202011341297 A CN202011341297 A CN 202011341297A CN 112358818 A CN112358818 A CN 112358818A
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J1/00—Adhesives based on inorganic constituents
- C09J1/02—Adhesives based on inorganic constituents containing water-soluble alkali silicates
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- Chemical & Material Sciences (AREA)
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- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
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Abstract
The invention provides a fireproof adhesive, which is prepared from the following raw materials: liquid sodium silicate, silica sol, polyvinyl alcohol, a defoaming agent, heat-absorbing powder, expanding powder, a dispersing agent, a wetting agent and fibers. The invention provides an inorganic-organic composite fireproof adhesive which can well bond a metal foil surface and an inorganic core material, has strong bonding force, obviously reduces the content of organic matters in the whole product, has the performance of releasing crystal water to reduce space temperature and thermal expansion, and can greatly improve the comprehensive fireproof capacity of the product. The fireproof glue provided by the invention can be applied to the fireproof in the power industry, and the fireproof material which is required to cover the metal foil in other industries can also be applied to the fireproof glue, so that the fireproof glue has a wide application range. The invention also provides a preparation method of the fireproof glue.
Description
Technical Field
The invention belongs to the technical field of fireproof materials, and particularly relates to a fireproof adhesive and a preparation method thereof.
Background
Key fire prevention parts of the power grid: the middle joint parts of the cable trench and the cable tunnel are fireproof and explosion-proof, and the fireproof walls of the cable trench and the cable tunnel are fireproof. The fire accident caused by explosion of the cable middle joint is a large proportion of the cable fire. After the cable joint is exploded and ignited, the cable joint has the serial ductility and serious ignition consequences, and particularly in high-risk places in production areas of industries such as nuclear power, thermal power generation, power transmission and transformation, petroleum and petrochemical industry and the like, the cable joint has high importance on cable fire protection of important circuits and cable middle joint parts.
At present, the cable is protected by adopting a fireproof coating material in international developed countries. The heat absorption type fire-proof wrapping roll is widely used due to its excellent fire-proof performance. The foreign representative product is a 3ME-Mat heat absorption type fireproof wrapping coiled material; however, when the aluminum foil is coated with the aluminum foil, the organic binder (acrylic resin) is adopted, so that the content of organic components of the whole product is increased, the comprehensive improvement of the fireproof performance of the product is not facilitated, and particularly, when the product catches fire in a closed space, more heat is released by the product in case of fire, so that the temperature of the space is increased rapidly.
Disclosure of Invention
In view of this, the present invention provides a fire-retardant adhesive and a preparation method thereof, and the fire-retardant adhesive provided by the present invention has a good fire-retardant capability.
The invention provides a fireproof adhesive, which is prepared from the following raw materials:
liquid sodium silicate, silica sol, polyvinyl alcohol, a defoaming agent, heat-absorbing powder, expanding powder, a dispersing agent, a wetting agent and fibers.
Preferably, the defoaming agent is selected from one or more of modified siloxane, organic silicon defoaming agent and mineral oil defoaming agent.
Preferably, the endothermic powder is selected from one or more of aluminum hydroxide, calcium carbonate, sodium bicarbonate, magnesium hydroxide and calcium hydroxide.
Preferably, the expanded powder material is selected from one or more of a mixture of dipentaerythritol and melamine, expandable graphite, vermiculite and expanded perlite.
Preferably, the fibers are selected from one or more of alumina fibers, ceramic fibers and glass fibers.
Preferably, the solid contents of the liquid sodium silicate, the silica sol, the polyvinyl alcohol, the defoaming agent, the heat absorbing powder, the expanding powder, the dispersing agent, the wetting agent and the fiber account for (6.5-8%) of the fireproof glue by mass percent: (4-5.5%): (0.5-1%): (0.5-1%): (35-40%): (24% -27%): (0.2-0.6%): (0.3-0.6%): (1.2% -1.5%).
The invention provides a preparation method of the fireproof adhesive, which comprises the following steps:
carrying out polymerization reaction on liquid sodium silicate, silica sol, polyvinyl alcohol and a defoaming agent, and then concentrating to obtain mixed sol;
and mixing the mixed sol, the heat absorption powder, the expansion powder, the fiber, the dispersing agent, the wetting agent and the defoaming agent to obtain the fireproof glue.
Preferably, the temperature of the polymerization reaction is 60-180 ℃.
Preferably, the vacuum degree of the concentration is 0.4-0.95 MPa.
Preferably, the viscosity of the mixed sol is 4000-7000 mpa.s (room temperature), and the solid content is 35-45%.
The invention provides an inorganic-organic composite fireproof adhesive and a preparation method thereof, the composite fireproof adhesive can well bond a metal foil surface and an inorganic core material, has stronger bonding force, obviously reduces the content of organic matters in the whole product, has the performance of releasing crystal water to reduce space temperature and thermal expansion, and can greatly improve the comprehensive fireproof capacity of the product. The fireproof glue provided by the invention can be applied to the fireproof in the power industry, and the fireproof material coated with the metal foil in other industries can also be applied to the fireproof glue, so that the fireproof glue has a wide application range.
Detailed Description
The technical solutions in the embodiments of the present invention will be 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 examples, which may be modified or appreciated by those of ordinary skill in the art based on the examples given herein, are intended to be within the scope of the present invention. It should be understood that the embodiments of the present invention are only for illustrating the technical effects of the present invention, and are not intended to limit the scope of the present invention. In the examples, the methods used were all conventional methods unless otherwise specified.
The invention provides a fireproof adhesive, which is prepared from the following raw materials:
liquid sodium silicate, silica sol, polyvinyl alcohol, a defoaming agent, heat-absorbing powder, expanding powder, a dispersing agent, a wetting agent and fibers.
The liquid sodium silicate is not particularly limited, and a commercially available product well known to those skilled in the art can be adopted, wherein the solid content of the liquid sodium silicate is preferably 25-35%, and more preferably 30%; the pH value of the liquid sodium silicate is preferably 9-10.
The silica sol is not particularly limited, and commercially available products well known to those skilled in the art can be adopted, wherein the solid content of the silica sol is preferably 20-30%, and more preferably 25%; the pH of the silica sol is preferably 9-10.
In the invention, the alcoholysis degree of the polyvinyl alcohol is preferably 88-99%, and more preferably 90-95%; the polymerization degree is preferably 1500 to 2000, more preferably 1600 to 1800. In the invention, the polyvinyl alcohol is preferably a polyvinyl alcohol solution, more preferably a polyvinyl alcohol aqueous solution, and the mass concentration of the polyvinyl alcohol solution is preferably 5-8%, more preferably 6-7%.
In the present invention, the defoaming agent is preferably one or more selected from modified siloxane, silicone defoaming agent and mineral oil defoaming agent, and more preferably polyether modified silicone oil.
In the invention, the granularity of the heat-absorbing powder is preferably 200-600 meshes, more preferably 300-500 meshes, and most preferably 350-450 meshes. In the present invention, the endothermic powder is preferably one or more selected from the group consisting of aluminum hydroxide, calcium carbonate, sodium bicarbonate, magnesium hydroxide and calcium hydroxide.
In the invention, the mass content of the heat-absorbing powder in the fireproof glue is preferably 35-40%.
In the present invention, the particle size of the expanded powder is preferably 80 to 600 mesh, more preferably 100 to 500 mesh, and most preferably 200 to 400 mesh. In the present invention, the expanded powder material is preferably selected from one or more of a mixture of dipentaerythritol and melamine, expandable graphite, vermiculite and expanded perlite. The bis-quaternary amylene alcohol and the melamine are not particularly limited in the invention, and can be commercially available products well known to those skilled in the art, and the mass ratio of the bis-quaternary amylene alcohol to the melamine is preferably (1-3): 1, more preferably (1.5 to 2.5): 1, most preferably 2: 1.
In the invention, the mass content of the expansion powder in the fireproof glue is preferably 24-27%.
In the present invention, the dispersant is preferably a polyamide epichlorohydrin resin.
The present invention is not particularly limited in the kind of the wetting agent, and a commercially available wetting agent known to those skilled in the art, such as Dow chemical 1211, may be used.
In the present invention, the fibers are preferably selected from one or more of alumina fibers, ceramic fibers and glass fibers. In the invention, the length of the fiber is preferably 4-5 mm, and the diameter of the fiber is preferably 3-5 microns.
In the invention, the mass content of the fiber in the fireproof glue is preferably 1.2-1.5%.
In the invention, the solid contents of the liquid sodium silicate, the silica sol, the polyvinyl alcohol, the defoaming agent, the heat absorbing powder, the expanding powder, the dispersing agent, the wetting agent and the fiber account for (6.5-8%) of the fireproof glue by mass percent: (4-5.5%): (0.5-1%): (0.5-1%): (35-40%): (24% -27%): (0.2-0.6%): (0.3-0.6%): (1.2% to 1.5%), more preferably (7% to 7.5%): (4.5-5%): (0.6-0.8%): (0.6-0.8%): (36-38%): (25-26%): (0.3-0.5%): (0.4-0.5%): (1.3% -1.4%).
The invention provides a preparation method of the fireproof glue in the technical scheme, which is prepared by adopting a sol-gel method and comprises the following steps:
carrying out polymerization reaction on liquid sodium silicate, silica sol, polyvinyl alcohol and a defoaming agent, and then concentrating to obtain mixed sol, wherein the defoaming agent is marked as a first defoaming agent;
and mixing the mixed sol, the heat absorption powder, the expansion powder, the fiber, the dispersing agent, the wetting agent and the defoaming agent to obtain the fireproof glue, and marking the defoaming agent as a second defoaming agent.
In the invention, the polymerization reaction temperature is preferably 60-180 ℃, more preferably 80-160 ℃, and most preferably 100-120 ℃; the polymerization reaction is preferably carried out under the condition of stirring, and the frequency of stirring is preferably 60-120 r/min, and more preferably 80-100 r/min.
In the invention, the concentration time is preferably 180-240 min, and more preferably 200-220 min; the vacuum degree of the concentration is preferably 0.4 to 0.95MPa, more preferably 0.5 to 0.9MPa, and most preferably 0.6 to 0.8 MPa.
In the invention, the viscosity of the mixed sol at room temperature is preferably 4000-7000 mpa.s, more preferably 5000-6000 mpa.s, and most preferably 5500 mpa.s; the solid content is preferably 35-45%, and more preferably 40%.
In the present invention, the mass ratio of the first defoaming agent to the second defoaming agent is preferably 1: (1.5-2), more preferably 1 (1.6-1.8).
In the present invention, the types and the amounts of the sodium silicate, the silica sol, the polyvinyl alcohol, the defoaming agent, the heat absorbing powder, the expanding powder, the fiber, the dispersing agent and the wetting agent are the same as those described in the above technical solution, and are not described herein again.
The fire-retardant adhesive provided by the invention has the following viscosity: 500-1500P; the solid content is more than 50 percent; fire performance grade a; the bonding strength is more than 0.2MPa, the core material and the metal foil are quickly dried within 1 hour after being bonded, the surface has no cracks, the content of inorganic components is high, the durability is good (irradiation resistance test), and the integrity is well maintained after the fiber is added and the fiber is burnt.
The invention provides an inorganic-organic composite fireproof adhesive and a preparation method thereof, the composite fireproof adhesive can well bond a metal foil surface and an inorganic core material, has stronger bonding force, obviously reduces the content of organic matters in the whole product, has the performance of releasing crystal water to reduce space temperature and thermal expansion, and can greatly improve the comprehensive fireproof capacity of the product. The fireproof glue provided by the invention can be applied to the fireproof in the power industry, and the fireproof material coated with the metal foil in other industries can also be applied to the fireproof glue, so that the fireproof glue has a wide application range.
The raw materials used in the following examples of the invention are all commercial products, the used liquid sodium silicate is provided by the Jinan original and easy environmental protection science and technology company, the silica sol is provided by the Qingdao ocean chemical company, the defoaming agent is a product of type B-157 provided by the middle federal company, the alumina fiber is provided by the Luyang energy-saving material GmbH, the polyamide epichlorohydrin resin is a product of type GC-19801 provided by the Shandong high energy-saving environmental protection science and technology GmbH, and 1211 is a product of the United states of Tao 1211.
Example 1
Weighing 700g of liquid sodium silicate (with the solid content of 25%) and 300g of silica sol (with the solid content of 30%), mixing, adding 265g of 7% polyvinyl alcohol (with the polymerization degree of 2000 and the alcoholysis degree of 99%) aqueous solution, adding 0.3g of defoaming agent, and carrying out concentration polymerization: the polymerization temperature is 130 ℃, the stirring frequency is 90r/min, the concentration time is 180min, the vacuum degree is 0.90MPa, and the sol with the viscosity of 5500mpa.s (room temperature) is obtained.
Mixing the sol, aluminum hydroxide, dipentaerythritol, melamine and alumina fibers to obtain slurry, wherein the mixing mass ratio is 32%: 37.7%: 18%: 9%: 1.5 percent of the fire-proof adhesive, then adding polyamide epichlorohydrin resin, 1211 and polyether modified silicone oil which respectively account for 0.6 percent of the total mass of the sizing agent, and uniformly stirring to obtain the fire-proof adhesive.
The viscosity of the fireproof adhesive prepared in the embodiment 1 of the invention is 1270P according to GB/T12954-; the solid content of the product is 81.3 percent after the product is burnt at 1000 ℃; bonding the fireproof glue with the metal foil and the fireproof core material, drying for 49min, and detecting the bonding strength of the fireproof glue to be 0.5MPa by using an HC-2000A type intelligent bonding strength detector; the fire-resistant material is detected to be A-grade fire-resistant according to GB/T GB8624-2012 'building material and product combustion performance grading', and the smoke is non-toxic; after being fired, the material is tightly adhered to the surface of the core material, and a layer of hard carbonized shell is formed on the surface.
Example 2
Weighing 700g of liquid sodium silicate and 300g of silica sol, mixing, adding 265g of 7% polyvinyl alcohol (polymerization degree 1700, alcoholysis degree 88%) aqueous solution, adding 0.3g of defoaming agent, and carrying out concentration polymerization: the polymerization temperature is 130 ℃, the stirring frequency is 90r/min, the concentration time is 200min, the vacuum degree is 0.95MPa, and sol is obtained, wherein the sol viscosity is 6700mpa.s (room temperature).
Mixing the sol, aluminum hydroxide, dipentaerythritol, melamine and aluminum oxide fibers to obtain slurry; the mixing mass ratio is 32%: 37.7%: 18%: 9%: 1.5 percent of the fire-proof adhesive, then adding polyamide epichlorohydrin resin, 1211 and polyether modified silicone oil which respectively account for 0.6 percent of the total mass of the sizing agent, and uniformly stirring to obtain the fire-proof adhesive.
The fire-proof adhesive prepared in the embodiment 2 of the invention is measured to have the viscosity of 1390P according to the method of the embodiment 1, and the solid content is 82.7 percent after being burnt at 1000 ℃; bonding the fireproof glue with the metal foil and the fireproof core material, drying for 44min, and detecting the bonding strength of the fireproof glue to be 0.38MPa by using an HC-2000A type intelligent bonding strength detector; the fire-resistant material is detected to be A-grade fire-resistant according to GB/T GB8624-2012 'building material and product combustion performance grading', and the smoke is non-toxic; after being fired, the material is tightly adhered to the surface of the core material, and a layer of hard carbonized shell is formed on the surface.
Comparative example 1
700g of liquid sodium silicate and 300g of silica sol are mixed, 265g of 7% polyvinyl alcohol (polymerization degree 2000, alcoholysis degree 99%) water solution by mass fraction is added, 0.3g of defoaming agent is added, and the mixture is uniformly stirred to obtain the sol.
Then mixing the sol, aluminum hydroxide, dipentaerythritol, melamine and aluminum oxide fibers to obtain slurry; the mixing mass ratio is 32%: 37.7%: 18%: 9%: 1.5 percent; then adding polyamide epichlorohydrin resin, 1211 and polyether modified silicone oil which respectively account for 0.6 percent of the total mass of the sizing agent, and uniformly stirring to obtain the fireproof glue.
Bonding the fireproof glue prepared in the comparative example 1 with a metal foil and a fireproof core material, wherein the drying time is 362min, and the bonding strength is detected to be 0.035MPa by using an HC-2000A type intelligent bonding strength detector; the solid content was found to be 28.9% after firing at 1000 ℃.
Comparative example 2
Weighing 700g of liquid sodium silicate and 300g of silica sol, mixing, adding 265g of 7% polyvinyl alcohol (polymerization degree 2000, alcoholysis degree 99%) aqueous solution, adding 0.3g of defoaming agent, and carrying out concentration polymerization: the polymerization temperature is 130 ℃, the stirring frequency is 90r/min, the concentration time is 180min, the vacuum degree is 0.90MPa, and the sol is obtained, and the viscosity of the sol is 5500mpa.s (room temperature).
Mixing the sol, alumina (1000 meshes), dipentaerythritol, melamine and alumina fibers to obtain slurry; the mixing mass ratio is 32%: 37.7%: 18%: 9%: 1.5 percent of the fire-proof adhesive, then adding polyamide epichlorohydrin resin, 1211 and polyether modified silicone oil which respectively account for 0.6 percent of the total mass of the sizing agent, and uniformly stirring to obtain the fire-proof adhesive.
The viscosity of the fire-proof adhesive prepared in comparative example 2 of the invention is 827P, and the solid content of the fire-proof adhesive is 82.3% after the fire-proof adhesive is burnt at 1000 ℃; bonding the fireproof adhesive with metal foil and fireproof core material, drying for 47min, and detecting adhesive strength of 0.32MPa with HC-2000A intelligent adhesive strength detector; the fire-resistant material is detected to be A-grade fire-resistant according to GB/T GB8624-2012 'building material and product combustion performance grading', and the smoke is non-toxic; after the coating dries, the coating shrinks seriously, the surface cracks and loses the fire-proof integrity.
The embodiment of the invention provides an inorganic-organic composite fireproof adhesive and a preparation method thereof, the composite fireproof adhesive can well bond a metal foil surface and an inorganic core material, has strong bonding force, obviously reduces the content of organic matters in the whole product, has the performance of releasing crystal water to reduce space temperature and thermal expansion, and can greatly improve the comprehensive fireproof capacity of the product. The fireproof glue provided by the invention can be applied to the fireproof in the power industry, and the fireproof material coated with the metal foil in other industries can also be applied to the fireproof glue, so that the fireproof glue has a wide application range.
While only the preferred embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (10)
1. The fireproof glue is prepared from the following raw materials:
liquid sodium silicate, silica sol, polyvinyl alcohol, a defoaming agent, heat-absorbing powder, expanding powder, a dispersing agent, a wetting agent and fibers.
2. The fire-retardant adhesive of claim 1, wherein the defoaming agent is one or more selected from modified siloxane, silicone defoaming agent and mineral oil defoaming agent.
3. The fireproof adhesive according to claim 1, wherein the heat-absorbing powder is selected from one or more of aluminum hydroxide, calcium carbonate, sodium bicarbonate, magnesium hydroxide and calcium hydroxide.
4. The fire-retardant adhesive according to claim 1, wherein the expanded powder material is one or more selected from the group consisting of a mixture of dipentaerythritol and melamine, expandable graphite, vermiculite and expanded perlite.
5. A fire-retardant adhesive according to claim 1, wherein the fibers are selected from one or more of alumina fibers, ceramic fibers and glass fibers.
6. The fireproof adhesive according to claim 1, wherein the solid contents of the liquid sodium silicate, the silica sol, the polyvinyl alcohol, the defoaming agent, the heat absorbing powder, the expanding powder, the dispersing agent, the wetting agent and the fiber account for (6.5-8%) of the fireproof adhesive by mass: (4-5.5%): (0.5-1%): (0.5-1%): (35-40%): (24% -27%): (0.2-0.6%): (0.3-0.6%): (1.2% -1.5%).
7. A method of preparing the fire-blocking glue of claim 1, comprising:
carrying out polymerization reaction on liquid sodium silicate, silica sol, polyvinyl alcohol and a defoaming agent, and then concentrating to obtain mixed sol;
and mixing the mixed sol, the heat absorption powder, the expansion powder, the fiber, the dispersing agent, the wetting agent and the defoaming agent to obtain the fireproof glue.
8. The process of claim 7, wherein the polymerization temperature is 60 to 180 ℃.
9. The method of claim 7, wherein the vacuum degree of the concentration is 0.4-0.95 MPa.
10. The method according to claim 7, wherein the mixed sol has a viscosity of 4000mpa.s to 7000mpa.s and a solid content of 35 to 45%.
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| CN113512363A (en) * | 2021-05-28 | 2021-10-19 | 海南大学 | Fireproof adhesive and preparation method thereof |
| WO2023154497A1 (en) * | 2022-02-11 | 2023-08-17 | Armstrong World Industries, Inc. | Fire resistant adhesive compositions and methods of preparing and using the same |
| US12018180B2 (en) | 2022-02-11 | 2024-06-25 | Awi Licensing Llc | Fire resistant adhesive compositions and methods of preparing and using the same |
| CN114958231A (en) * | 2022-06-17 | 2022-08-30 | 广东粤港澳大湾区国家纳米科技创新研究院 | Fireproof adhesive tape and preparation method and application thereof |
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