CN117866510A - High-temperature aerogel heat-insulating fireproof coating and preparation method thereof - Google Patents

High-temperature aerogel heat-insulating fireproof coating and preparation method thereof Download PDF

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Publication number
CN117866510A
CN117866510A CN202410056218.2A CN202410056218A CN117866510A CN 117866510 A CN117866510 A CN 117866510A CN 202410056218 A CN202410056218 A CN 202410056218A CN 117866510 A CN117866510 A CN 117866510A
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parts
temperature
fireproof coating
aerogel heat
heat
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CN202410056218.2A
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Chinese (zh)
Inventor
常文涛
李宁
陈静
刘超旭
袁啸天
窦可
张栋
楚雪靖
徐建
李雪梅
范丽娜
宋笑育
张永梅
杜艳群
毕建亮
李苏豫
刘盼盼
吕梦凡
袁铁锁
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Henan Meida Industrial Co ltd
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Henan Meida Industrial Co ltd
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Priority to CN202410056218.2A priority Critical patent/CN117866510A/en
Publication of CN117866510A publication Critical patent/CN117866510A/en
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Abstract

The invention provides a high-temperature aerogel heat-insulating fireproof coating and a preparation method thereof, wherein the high-temperature aerogel heat-insulating fireproof coating comprises the following raw materials in parts by weight: 10-20 parts of high-temperature-resistant inorganic fibers, 40-60 parts of silicon source precursors, 80-100 parts of solvents, 10-20 parts of epoxybromobutane, 10-20 parts of dimethyl nitrite sodium, 10-20 parts of hydrogen chloride, 40-60 parts of binders, 10-20 parts of hard calcium silicate plates and 5-15 parts of ammonia water. The invention improves the porosity of the high-temperature aerogel heat-insulating fireproof coating, so that the aerogel heat-insulating fireproof coating has excellent heat-insulating performance, flame-retardant performance, corrosion resistance and heat-insulating performance.

Description

High-temperature aerogel heat-insulating fireproof coating and preparation method thereof
Technical Field
The invention relates to the technical field of fireproof coatings, in particular to a high-temperature aerogel heat-insulating fireproof coating and a preparation method thereof.
Background
The aerogel coating belongs to a composite heat-insulating fireproof coating, and utilizes the nano-pore structure and formula adjustment of the aerogel material to reduce heat conduction, heat convection and heat radiation, improve the overall heat insulation performance of the heat-insulating coating, and has pure inorganic components, so that the heat-resistant grade of 1000 ℃ can be achieved, and the heat-resistant and efficient heat insulation functions are integrated. The aerogel coating is one of the best heat insulation coatings at present, is a product in a true nano pore level, and can greatly improve the anti-radiation heat performance by adding a proper anti-radiation component into a coating formula; because the aperture of the nano-pore is small enough and smaller than the free path of air molecules, air convection cannot effectively occur; therefore, the nano-scale heat insulation material has excellent comprehensive heat insulation performance.
The aerogel powder has a unique nano-pore structure and extremely low density, and can block heat transfer from three aspects of heat conduction, heat radiation and heat convection. SiO (SiO) 2 Aerogels are the usual aerogel types, siO 2 The internal structure of aerogel is complex and changeable, which results in very complex heat transfer process, and thermal conductivity and thermal insulation performance are to be improved, so that improvement of aerogel in related technology is needed.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a high-temperature aerogel heat-insulating fireproof coating and a preparation method thereof, and the high-temperature aerogel heat-insulating fireproof coating can be used.
In order to achieve the above purpose, the invention is realized by the following technical scheme:
the high-temperature aerogel heat-insulating fireproof paint comprises the following raw materials in parts by weight: 10-20 parts of high-temperature-resistant inorganic fibers, 40-60 parts of silicon source precursors, 80-100 parts of solvents, 10-20 parts of epoxybromobutane, 10-20 parts of dimethyl nitrite sodium, 10-20 parts of hydrogen chloride, 40-60 parts of binders, 10-20 parts of hard calcium silicate plates and 5-15 parts of ammonia water.
Preferably, the fireproof coating comprises the following raw materials in parts by weight: 15 parts of high-temperature-resistant inorganic fibers, 50 parts of silicon source precursors, 90 parts of solvents, 15 parts of epoxybromobutane, 15 parts of dimethyl sodium nitrite, 15 parts of hydrogen chloride, 50 parts of binders, 15 parts of hard silicon calcium plates and 10 parts of ammonia water.
Preferably, the high-temperature-resistant inorganic fiber is one of aluminum silicate fiber, nitrogen-lao-boron fiber or carbon fiber.
Preferably, the silicon source precursor is one of trimethylchlorosilane, hexamethyldisilazane, methyltrimethoxysilane, methyl orthosilicate, water glass, fluorosilane or tetramethoxysilane.
Preferably, the solvent is one of absolute alcohol, n-hexane or isopropanol.
Preferably, the binder is one of an epoxy resin emulsion, an acrylic resin emulsion, or a silicone resin emulsion.
Preferably, the preparation method of the high-temperature aerogel heat-insulating fireproof coating comprises the following steps: .
Preferably, said.
The preparation method of the high-temperature aerogel heat-insulating fireproof coating comprises the following steps:
s1, weighing dimethyl sodium nitrite and epoxybromobutane according to a proportion, reacting for 1-2 hours at 50-55 ℃, then adding a proper amount of hydrogen chloride until the solution is neutral, distilling, and then suction-filtering to obtain (3-chloro-2-hydroxy) propyl dimethyl nitrate;
s2, weighing a silicon source precursor, 1/2 mass of solvent and ammonia water according to a proportion, adding the rest hydrogen chloride, and then adding the ammonia water to prepare SiO2 sol;
s3, weighing the rest raw materials according to a proportion, uniformly mixing the rest raw materials with (3-chloro-2-hydroxy) propyl dimethyl nitrate and SiO2 sol, adding the mixture into a vacuum device, and opening a vacuum valve after 1-2 hours to obtain the finished product.
Preferably, the pressure in the vacuum device is 0.5-1MPa.
The beneficial effects of the invention are as follows:
novel composite heat-insulating material with xonotlite as reinforced skeleton for better SiO 2 Aerogel, high temperature resistant inorganic fiber and xonotlite particles are compounded, the application adopts vacuum impregnation technology, siO 2 Aerogel and high temperature resistant inorganic fiber and tobermorite are compounded to formThe intertwined and interwoven hollow sphere granular aggregate has the characteristics of high porosity and low density, and improves the porosity of the high-temperature aerogel heat-insulating fireproof coating, so that the high-temperature aerogel heat-insulating fireproof coating has excellent heat-insulating performance.
The sodium dimethyl nitrite and the epoxybromobutane react with hydrogen chloride to generate (3-chloro-2-hydroxy) propyl dimethyl nitrate, and the (3-chloro-2-hydroxy) propyl dimethyl nitrate contains two elements of nitrogen and bromine, so that the flame retardant coating has good flame retardant property, is used for preparing high-temperature aerogel heat-insulating fireproof coating, and has good flame retardant property.
SiO prepared from a silicon source precursor 2 The reticular structure formed after the aerogel is dispersed effectively enhances the strength of the coating, the surface hydrophobicity further hinders the infiltration of corrosive medium, and the corrosion resistance of the coating is improved.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1:
the embodiment discloses a high-temperature aerogel heat-insulating fireproof coating, which is prepared from the following raw materials in proportion: 10 parts of high-temperature-resistant inorganic fibers, 40 parts of silicon source precursors, 80 parts of solvents, 10 parts of epoxybromobutane, 10 parts of dimethyl sodium nitrite, 10 parts of hydrogen chloride, 40 parts of binders, 10 parts of hard silicon calcium plates and 5 parts of ammonia water.
Wherein the high temperature resistant inorganic fiber is aluminum silicate fiber.
The silicon source precursor is trimethylchlorosilane.
The solvent is anhydrous alcohol.
The binder is an epoxy resin emulsion.
The preparation method of the high-temperature aerogel heat-insulating fireproof coating comprises the following steps:
s1, weighing dimethyl sodium nitrite and epoxybromobutane according to a proportion, reacting for 1h at 50 ℃, then adding a proper amount of hydrogen chloride until the solution is neutral, distilling, and suction-filtering to obtain (3-chloro-2-hydroxy) propyl dimethyl nitrate;
s2, weighing a silicon source precursor, 1/2 mass of solvent and ammonia water according to a proportion, adding the rest hydrogen chloride, and then adding the ammonia water to prepare SiO 2 Sol;
s3, weighing the rest raw materials in proportion, and mixing the rest raw materials with (3-chloro-2-hydroxy) propyl dimethyl nitrate and SiO 2 And (3) uniformly mixing the sol, adding the mixture into a vacuum device of 0.5MPa, and opening a vacuum valve after 1h to obtain the sol.
Example 2:
the embodiment discloses a high-temperature aerogel heat-insulating fireproof coating, which is prepared from the following raw materials in proportion: 20 parts of high-temperature-resistant inorganic fibers, 60 parts of silicon source precursors, 100 parts of solvents, 20 parts of epoxybromobutane, 20 parts of dimethyl sodium nitrite, 20 parts of hydrogen chloride, 60 parts of binders, 20 parts of hard calcium silicate plates and 15 parts of ammonia water.
Wherein the high temperature resistant inorganic fiber is a nitrogen-Lao-boron fiber.
The silicon source precursor is hexamethyldisilazane.
The solvent was n-hexane.
The binder is acrylic resin emulsion.
The preparation method of the high-temperature aerogel heat-insulating fireproof coating comprises the following steps:
s1, weighing dimethyl sodium nitrite and epoxybromobutane according to a proportion, reacting for 2 hours at 55 ℃, then adding a proper amount of hydrogen chloride until the solution is neutral, distilling, and suction-filtering to obtain (3-chloro-2-hydroxy) propyl dimethyl nitrate;
s2, weighing a silicon source precursor, 1/2 mass of solvent and ammonia water according to a proportion, adding the rest hydrogen chloride, and then adding the ammonia water to prepare SiO 2 Sol;
s3, weighing the rest raw materials in proportion, and mixing the rest raw materials with (3-chloro-2-hydroxy) propyl dimethyl nitrate and SiO 2 Sol-gelAnd (3) uniformly mixing, adding the mixture into a vacuum device of 1MPa, and opening a vacuum valve after 2 hours to obtain the product.
Example 3:
the embodiment discloses a high-temperature aerogel heat-insulating fireproof coating, which is prepared from the following raw materials in proportion: 15 parts of high-temperature-resistant inorganic fibers, 50 parts of silicon source precursors, 90 parts of solvents, 15 parts of epoxybromobutane, 15 parts of dimethyl sodium nitrite, 15 parts of hydrogen chloride, 50 parts of binders, 15 parts of hard silicon calcium plates and 10 parts of ammonia water.
Wherein the high temperature resistant inorganic fiber is carbon fiber.
A silicon source precursor methyltrimethoxysilane.
The solvent is isopropanol.
The binder ring is a silicone resin emulsion.
The preparation method of the high-temperature aerogel heat-insulating fireproof coating comprises the following steps:
s1, weighing dimethyl sodium nitrite and epoxybromobutane according to a proportion, reacting for 1h at 50 ℃, then adding a proper amount of hydrogen chloride until the solution is neutral, distilling, and suction-filtering to obtain (3-chloro-2-hydroxy) propyl dimethyl nitrate;
s2, weighing a silicon source precursor, 1/2 mass of solvent and ammonia water according to a proportion, adding the rest hydrogen chloride, and then adding the ammonia water to prepare SiO 2 Sol;
s3, weighing the rest raw materials in proportion, and mixing the rest raw materials with (3-chloro-2-hydroxy) propyl dimethyl nitrate and SiO 2 And (3) uniformly mixing the sol, adding the mixture into a vacuum device of 0.5MPa, and opening a vacuum valve after 1h to obtain the sol.
Example 4:
the embodiment discloses a high-temperature aerogel heat-insulating fireproof coating, which is prepared from the following raw materials in proportion: 14 parts of high-temperature-resistant inorganic fibers, 46 parts of a silicon source precursor, 86 parts of a solvent, 14 parts of epoxybromobutane, 14 parts of dimethyl sodium nitrite, 14 parts of hydrogen chloride, 46 parts of a binder, 14 parts of a hard silicon calcium plate and 8 parts of ammonia water.
Wherein the high temperature resistant inorganic fiber is aluminum silicate fiber.
The silicon source precursor is methyl orthosilicate.
The solvent is anhydrous alcohol.
An adhesive epoxy resin emulsion.
The preparation method of the high-temperature aerogel heat-insulating fireproof coating comprises the following steps:
s1, weighing dimethyl sodium nitrite and epoxybromobutane according to a proportion, reacting for 2 hours at 55 ℃, then adding a proper amount of hydrogen chloride until the solution is neutral, distilling, and suction-filtering to obtain (3-chloro-2-hydroxy) propyl dimethyl nitrate;
s2, weighing a silicon source precursor, 1/2 mass of solvent and ammonia water according to a proportion, adding the rest hydrogen chloride, and then adding the ammonia water to prepare SiO 2 Sol;
s3, weighing the rest raw materials in proportion, and mixing the rest raw materials with (3-chloro-2-hydroxy) propyl dimethyl nitrate and SiO 2 And (3) uniformly mixing the sol, adding the mixture into a vacuum device of 0.5MPa, and opening a vacuum valve after 1h to obtain the sol.
Example 5:
the embodiment discloses a high-temperature aerogel heat-insulating fireproof coating, which is prepared from the following raw materials in proportion: 18 parts of high-temperature-resistant inorganic fibers, 54 parts of a silicon source precursor, 94 parts of a solvent, 16 parts of epoxybromobutane, 16 parts of dimethyl sodium nitrite, 16 parts of hydrogen chloride, 54 parts of a binder, 16 parts of a hard silicon calcium plate and 12 parts of ammonia water.
Wherein the high temperature resistant inorganic fiber is aluminum silicate fiber.
The silicon source precursor is water glass.
The solvent is anhydrous alcohol.
An adhesive epoxy resin emulsion.
The preparation method of the high-temperature aerogel heat-insulating fireproof coating comprises the following steps:
s1, weighing dimethyl sodium nitrite and epoxybromobutane according to a proportion, reacting for 2 hours at 55 ℃, then adding a proper amount of hydrogen chloride until the solution is neutral, distilling, and suction-filtering to obtain (3-chloro-2-hydroxy) propyl dimethyl nitrate;
s2, weighing a silicon source precursor, 1/2 mass of solvent and ammonia water according to a proportion, and adding the rest chlorineHydrogen chloride, and ammonia water are added to prepare SiO 2 Sol;
s3, weighing the rest raw materials in proportion, and mixing the rest raw materials with (3-chloro-2-hydroxy) propyl dimethyl nitrate and SiO 2 And (3) uniformly mixing the sol, adding the mixture into a vacuum device of 1MPa, and opening a vacuum valve after 2 hours to obtain the sol.
Comparative example 1:
a high temperature aerogel thermal insulation fire retardant coating differing from example 3 only in that: no high temperature resistant inorganic fiber is added.
Comparative example 2:
a high temperature aerogel thermal insulation fire retardant coating differing from example 3 only in that: no oxybutylene was added.
Comparative example 3:
a high temperature aerogel thermal insulation fire retardant coating differing from example 3 only in that: sodium dimethyl nitrite was not added.
Comparative example 4:
a high temperature aerogel thermal insulation fire retardant coating differing from example 3 only in that: no hydrogen chloride was added.
Comparative example 5:
a high temperature aerogel thermal insulation fire retardant coating differing from example 3 only in that: no hard calcium silicate board was added.
Comparative example 6:
a high temperature aerogel thermal insulation fire retardant coating differing from example 3 only in that: ammonia was not added.
The fireproof coatings obtained in examples 1 to 5 and comparative examples 1 to 6 were subjected to performance test, and the comprehensive properties in the fireproof coatings were measured, and the results are shown in Table 1.
TABLE 1 Performance parameters of the fire-retardant coatings obtained in examples 1-5, comparative examples 1-6
As can be seen from table 1:
the heat insulation performance of the fireproof paint can be slightly affected by no high-temperature-resistant inorganic fiber, epoxybromobutane, sodium dimethyl nitrite and hydrogen chloride.
The absence of the silicon source precursor can have a severe impact on the thermal insulation properties and fire rating of the fire retardant coating.
Ammonia water is not added, so that the heat insulation performance of the fireproof paint is not greatly influenced.
In summary, the xonotlite is a novel composite heat-insulating material with a reinforced framework, in order to better enable SiO2 aerogel, high-temperature-resistant inorganic fibers and xonotlite particles to be compounded, the application adopts a vacuum impregnation technology, and the SiO2 aerogel, the high-temperature-resistant inorganic fibers and the xonotlite are compounded to form a hollow spherical granular aggregate which is intertwined and interweaved, so that the novel composite heat-insulating material has the characteristics of high porosity and low density, and the porosity of the high-temperature aerogel heat-insulating fireproof coating is improved, so that the novel composite heat-insulating material has excellent heat-insulating performance.
The sodium dimethyl nitrite and the epoxybromobutane react with hydrogen chloride to generate (3-chloro-2-hydroxy) propyl dimethyl nitrate, and the (3-chloro-2-hydroxy) propyl dimethyl nitrate contains two elements of nitrogen and bromine, so that the flame retardant coating has good flame retardant property, is used for preparing high-temperature aerogel heat-insulating fireproof coating, and has good flame retardant property.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims (8)

1. The high-temperature aerogel heat-insulating fireproof coating is characterized by comprising the following raw materials in parts by weight: 10-20 parts of high-temperature-resistant inorganic fibers, 40-60 parts of silicon source precursors, 80-100 parts of solvents, 10-20 parts of epoxybromobutane, 10-20 parts of dimethyl nitrite sodium, 10-20 parts of hydrogen chloride, 40-60 parts of binders, 10-20 parts of hard calcium silicate plates and 5-15 parts of ammonia water.
2. The high-temperature aerogel heat-insulating fireproof coating according to claim 1, wherein the fireproof coating comprises the following raw materials in parts by weight: 15 parts of high-temperature-resistant inorganic fibers, 50 parts of silicon source precursors, 90 parts of solvents, 15 parts of epoxybromobutane, 15 parts of dimethyl sodium nitrite, 15 parts of hydrogen chloride, 50 parts of binders, 15 parts of hard silicon calcium plates and 10 parts of ammonia water.
3. The high-temperature aerogel heat-insulating fireproof coating according to claim 1 or 2, wherein the high-temperature-resistant inorganic fiber is one of aluminum silicate fiber, nitrogen-lao-boron fiber or carbon fiber.
4. The high temperature aerogel thermal insulation fire retardant coating of claim 1 or 2, wherein the silicon source precursor is one of trimethylchlorosilane, hexamethyldisilazane, methyltrimethoxysilane, methyl orthosilicate, water glass, fluorosilane, or tetramethoxysilane.
5. The high temperature aerogel heat insulation fire retardant coating of claim 4, wherein the solvent is one of absolute alcohol, n-hexane or isopropanol.
6. The high temperature aerogel thermal insulation fire retardant coating of claim 4, wherein the binder is one of an epoxy resin emulsion, an acrylic resin emulsion, or a silicone resin emulsion.
7. The high-temperature aerogel heat-insulating fireproof coating according to claim 4, wherein the preparation method of the fireproof coating comprises the following steps:
s1, weighing dimethyl sodium nitrite and epoxybromobutane according to a proportion, reacting for 1-2 hours at 50-55 ℃, then adding a proper amount of hydrogen chloride until the solution is neutral, distilling, and then suction-filtering to obtain (3-chloro-2-hydroxy) propyl dimethyl nitrate;
s2, weighing a silicon source precursor, 1/2 mass of solvent and ammonia water according to a proportion, adding the rest hydrogen chloride, and then adding the ammonia water to prepare SiO 2 Sol;
s3, weighing the rest raw materials in proportion, and mixing the rest raw materials with (3-chloro-2-hydroxy) propyl dimethyl nitrate and SiO 2 And (5) uniformly mixing the sol, adding the mixture into a vacuum device, and opening a vacuum valve after 1 to 2 hours to obtain the sol.
8. The high temperature aerogel heat insulation fire retardant coating of claim 7, wherein the pressure in the vacuum device is 0.5-1MPa.
CN202410056218.2A 2024-01-15 2024-01-15 High-temperature aerogel heat-insulating fireproof coating and preparation method thereof Pending CN117866510A (en)

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