CN116002693B - Flame-retardant silica aerogel and preparation method and application thereof - Google Patents
Flame-retardant silica aerogel and preparation method and application thereof Download PDFInfo
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- CN116002693B CN116002693B CN202211735131.5A CN202211735131A CN116002693B CN 116002693 B CN116002693 B CN 116002693B CN 202211735131 A CN202211735131 A CN 202211735131A CN 116002693 B CN116002693 B CN 116002693B
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 121
- 239000003063 flame retardant Substances 0.000 title claims abstract description 59
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000004965 Silica aerogel Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 32
- 239000002904 solvent Substances 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 27
- 238000000576 coating method Methods 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 12
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 9
- 230000032683 aging Effects 0.000 claims abstract description 8
- 150000007522 mineralic acids Chemical class 0.000 claims abstract description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 28
- 239000011240 wet gel Substances 0.000 claims description 28
- 239000011259 mixed solution Substances 0.000 claims description 24
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 22
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 11
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- 239000003377 acid catalyst Substances 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 229920001276 ammonium polyphosphate Polymers 0.000 claims description 6
- 239000004114 Ammonium polyphosphate Substances 0.000 claims description 5
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 claims 1
- 239000004964 aerogel Substances 0.000 abstract description 9
- 239000003054 catalyst Substances 0.000 abstract description 7
- 239000003973 paint Substances 0.000 abstract description 7
- 238000009413 insulation Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 3
- UIUXUFNYAYAMOE-UHFFFAOYSA-N methylsilane Chemical compound [SiH3]C UIUXUFNYAYAMOE-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract description 2
- 239000011248 coating agent Substances 0.000 description 13
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 229910004298 SiO 2 Inorganic materials 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 239000000499 gel Substances 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229920000877 Melamine resin Polymers 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 230000001680 brushing effect Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 244000137852 Petrea volubilis Species 0.000 description 1
- 229920000388 Polyphosphate Polymers 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000007171 acid catalysis Methods 0.000 description 1
- 238000005903 acid hydrolysis reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- -1 fluoride ions Chemical class 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000012767 functional filler Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000001205 polyphosphate Substances 0.000 description 1
- 235000011176 polyphosphates Nutrition 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
The invention discloses a flame-retardant silicon dioxide aerogel and a preparation method and application thereof. According to the invention, water glass and methylsilane are used as precursors, inorganic acid is used as a catalyst, a flame retardant is added in the gelling process, and the flame retardant silica aerogel is prepared after aging, solvent replacement and normal-pressure drying and is further applied to fireproof paint. The flame-retardant silica aerogel provided by the invention has the advantages of simple method, low density and good heat insulation effect, and meanwhile, the addition of the flame retardant improves the thermal stability of the material, achieves good flame-retardant effect, and is particularly suitable for being applied to fireproof coatings.
Description
Technical Field
The invention belongs to the technical field of silica aerogel, and particularly relates to flame-retardant silica aerogel, a preparation method thereof and application thereof in fireproof paint.
Background
SiO 2 aerogel is a high-dispersion solid material which is formed by mutually gathering nano-scale particles to form a nano-porous network structure and is filled with gaseous dispersion medium in pores, and has the characteristics of nano-porous structure, low density, low dielectric constant, low heat conductivity, high porosity, high specific surface area and the like, thus showing unique properties in mechanical, acoustic, thermal, optical and other aspects, and having wide and huge application value in various fields of aerospace, military, petroleum, chemical industry, mineral products, communication, medical, building materials, electronics, metallurgy and the like, and being called as a world-changing magic material.
At present, the preparation of the silica aerogel is mainly carried out by a chemical method, namely, in a specific solvent, under the combined action of water and a catalyst, a silicon source is hydrolyzed and polycondensed to form wet gel, and the wet gel is aged, modified and dried to obtain the silica aerogel. Therefore, the preparation process of the silicon dioxide aerogel is optimized from the aspects of a silicon source, a solvent, a catalyst, a modifier, a drying method and the like, and the low-cost rapid preparation of the aerogel material is a development trend for realizing the large-scale industrial production of the SiO 2 aerogel.
The SiO 2 aerogel fireproof paint takes SiO 2 aerogel as a functional filler, is uniformly dispersed in a stable system of the paint, and effectively plays a good heat insulation protection role by means of extremely low heat conductivity coefficient of the silica aerogel and the binding role of the pore diameter of the silica aerogel on air molecules, so that the fire resistance of the silica aerogel is improved, and the fireproof role is played. It is generally believed that SiO 2 aerogel itself is an inorganic filler that has certain flame retardant properties and thus contributes to the flame retardance of the coating. However, the preparation of silica aerogel at normal pressure and the relatively sufficient surface modification of silica are necessary conditions for preparing porous silica aerogel having excellent hydrophobicity and dispersibility. And a large amount of organic groups introduced by surface modification are heated and decomposed at high temperature to release a large amount of combustible gas, so that the combustion characteristics of the silica aerogel are changed to a certain extent. The oxygen index of the silica aerogel sold on the market is mostly below 25 through tests, and the silica aerogel belongs to the category of combustibles. Therefore, it is necessary to perform flame retardant modification on the silica aerogel prepared by the normal pressure method so as to improve the flame retardant property of the silica aerogel in the fireproof coating material.
Disclosure of Invention
The invention aims to effectively solve the problems and provides a flame-retardant silica aerogel and a preparation method and application thereof.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the preparation method of the flame-retardant silica aerogel comprises the following steps:
(1) Uniformly mixing water glass and deionized water at room temperature, adding Hexamethyldisilazane (HMDS) and n-hexane, and uniformly stirring to obtain a mixed solution;
(2) Adding an inorganic acid catalyst and a flame retardant into the mixed solution, uniformly stirring, adding ammonia water to adjust the pH to be 8-9, standing for 0.5-2 h at room temperature, and removing a water layer after layering the solution to obtain a silica wet gel;
wherein the inorganic acid catalyst is a mixture of phosphoric acid and hydrofluoric acid;
(3) Aging the silica wet gel at room temperature for at least 24 hours, and respectively performing solvent replacement in ethanol and n-hexane;
(4) And drying the silica wet gel subjected to solvent replacement at normal pressure to obtain the flame-retardant silica aerogel.
In the step (1), the mass ratio of the water glass to the deionized water to the hexamethyldisilazane to the n-hexane in the mixed solution is 1:3-5:0.2-2:3-15.
In the step (2), the inorganic acid catalyst accounts for 2-10% of the total mass of the mixed solution, and the flame retardant accounts for 0.5-1.5% of the total mass of the mixed solution.
In the step (2), the mass ratio of phosphoric acid to hydrofluoric acid in the inorganic acid catalysis is 1-3:1.
In the step (2), the flame retardant is one or more of melamine, pentaerythritol, ammonium polyphosphate and melamine polyphosphate.
In the step (3), the solvent replacement method is to soak the silica wet gel in the corresponding solvent at room temperature for 24-72 h.
In the step (4), the normal pressure drying treatment method comprises the following steps: the silica wet gel after solvent replacement is dried for 2 to 6 hours at normal pressure under the environment of 50 ℃, 80 ℃, 110 ℃, 150 ℃ and 180 ℃ respectively, and then naturally cooled to 25 ℃.
The heat conductivity coefficient of the flame-retardant silica aerogel prepared by the method is 0.02-0.05W/mK, the water contact angle is more than 120 degrees, and the oxygen index is more than or equal to 28.
The flame-retardant silica aerogel can be applied to fireproof coatings.
According to the invention, sodium silicate and methylsilane are used as precursors, phosphoric acid and hydrofluoric acid are used as composite catalysts, a flame retardant is added in the gelling process, and after aging and solvent replacement, the flame retardant silica aerogel is prepared by drying under normal pressure, and is further applied to fireproof paint.
The invention has the following beneficial effects:
1. The invention takes phosphoric acid and hydrofluoric acid as catalysts, wherein fluoride ions in the hydrofluoric acid play a role in catalytic crosslinking in the synthesis process of the silicon dioxide aerogel, and compared with the acid-base catalysts commonly used at present, the invention has the advantages of high catalytic efficiency, short required time, simple operation process and the like by using fluoride ion catalysis. The phosphoric acid plays a role in acidic hydrolysis of a silicon source and coordination stabilization of F ions, and also has a certain flame retardant effect, so that the subsequent flame retardant treatment is facilitated.
2. According to the invention, the organic flame retardant is introduced into the silica aerogel, so that the problem of flammability of the silica aerogel caused by hydrophobic modification is solved, and meanwhile, the hydrophobic silica aerogel carrier flame retardant can be uniformly dispersed in a coating material, so that the flame retardant effect is improved.
Detailed Description
The following examples will enable those skilled in the art to better understand the present invention and are not intended to limit the same in any way.
The proportions of the components added in the examples are parts by weight unless otherwise indicated.
Example 1
Preparation of flame retardant silica aerogel
(1) Uniformly mixing 10 parts of water glass with 30 parts of deionized water at room temperature, adding 10 parts of Hexamethyldisilazane (HMDS) and 30 parts of n-hexane, and uniformly stirring to obtain a mixed solution;
(2) Adding a mixed solution of phosphoric acid and hydrofluoric acid with the mass ratio of 2:1 and ammonium polyphosphate flame retardant with the mass ratio of 0.5% of the total mass of the mixed solution into the mixed solution, uniformly stirring, adding ammonia water to adjust the pH value to be 8.5, standing for 1h at room temperature, layering the solution, and removing a water layer to obtain a silica wet gel;
(3) Aging the silica wet gel for 24 hours at room temperature, and respectively carrying out solvent replacement in ethanol and n-hexane, wherein the solvent replacement method is to soak the silica wet gel in a corresponding solvent at room temperature for 48 hours;
(4) And respectively drying the silica wet gel subjected to solvent replacement at 50 ℃, 80 ℃, 110 ℃, 150 ℃ and 180 ℃ for 2-6 hours under normal pressure, and naturally cooling to 25 ℃ to obtain the flame-retardant silica aerogel.
The flame-retardant silica aerogel prepared according to the method has a thermal conductivity of 0.038W/mK, a water contact angle of 125 degrees and an oxygen index of 29.
Example 2
Preparation of flame retardant silica aerogel
(1) Uniformly mixing 10 parts of water glass with 35 parts of deionized water at room temperature, adding 10 parts of Hexamethyldisilazane (HMDS) and 30 parts of n-hexane, and uniformly stirring to obtain a mixed solution;
(2) Adding a mixed solution of phosphoric acid and hydrofluoric acid with the mass ratio of 1:1 and ammonium polyphosphate flame retardant with the mass ratio of 1% of the total mass of the mixed solution into the mixed solution, uniformly stirring, adding ammonia water to adjust the pH value to be 8, standing for 1h at room temperature, layering the solution, and removing a water layer to obtain a silica wet gel;
(3) Aging the silica wet gel for 24 hours at room temperature, and respectively carrying out solvent replacement in ethanol and n-hexane, wherein the solvent replacement method is to soak the silica wet gel in a corresponding solvent at room temperature for 48 hours;
(4) And respectively drying the silica wet gel subjected to solvent replacement at 50 ℃, 80 ℃, 110 ℃, 150 ℃ and 180 ℃ for 2-6 hours under normal pressure, and naturally cooling to 25 ℃ to obtain the flame-retardant silica aerogel.
The flame-retardant silica aerogel prepared according to the method has a heat conductivity coefficient of 0.027W/mK, a water contact angle of 135 degrees and an oxygen index of 28.
Example 3
Preparation of flame retardant silica aerogel
(1) Uniformly mixing 10 parts of water glass with 30 parts of deionized water at room temperature, adding 20 parts of Hexamethyldisilazane (HMDS) and 30 parts of n-hexane, and uniformly stirring to obtain a mixed solution;
(2) Adding a mixed solution of phosphoric acid and hydrofluoric acid with the mass ratio of 1:1 and ammonium polyphosphate flame retardant with the mass ratio of 1.5% of the total mass of the mixed solution into the mixed solution, uniformly stirring, adding ammonia water to adjust the pH value to be 9, standing for 1h at room temperature, layering the solution, and removing a water layer to obtain a silica wet gel;
(3) Aging the silica wet gel for 24 hours at room temperature, and respectively carrying out solvent replacement in ethanol and n-hexane, wherein the solvent replacement method is to soak the silica wet gel in a corresponding solvent at room temperature for 48 hours;
(4) And respectively drying the silica wet gel subjected to solvent replacement at 50 ℃, 80 ℃, 110 ℃, 150 ℃ and 180 ℃ for 2-6 hours under normal pressure, and naturally cooling to 25 ℃ to obtain the flame-retardant silica aerogel.
The flame-retardant silica aerogel prepared by the method has a heat conductivity coefficient of 0.031W/mK, a water contact angle of 142 degrees and an oxygen index of 28.
Comparative example 1
Preparation of silica aerogel
(1) Uniformly mixing 10 parts of water glass with 30 parts of deionized water at room temperature, adding 10 parts of Hexamethyldisilazane (HMDS) and 30 parts of n-hexane, and uniformly stirring to obtain a mixed solution;
(2) Adding sulfuric acid solution with the total mass of 5% into the mixed solution, uniformly stirring, hydrolyzing for 3 hours, adding ammonia water to adjust the pH=8.5, standing for gel for 6-8 hours at room temperature, layering the solution, and removing a water layer to obtain silica wet gel;
(3) Aging the silica wet gel for 24 hours at room temperature, and respectively carrying out solvent replacement in ethanol and n-hexane, wherein the solvent replacement method is to soak the silica wet gel in a corresponding solvent at room temperature for 48 hours;
(4) And respectively drying the silica wet gel subjected to solvent replacement at 50 ℃, 80 ℃, 110 ℃, 150 ℃ and 180 ℃ for 2-6 hours under normal pressure, and naturally cooling to 25 ℃ to obtain the silica aerogel.
The silica aerogel prepared according to the above method had a thermal conductivity of 0.025W/mK, a water contact angle of 121℃and an oxygen index of 23.
As can be seen from the above examples and comparative examples: (1) The mixed catalyst of phosphoric acid and hydrofluoric acid greatly reduces the hydrolysis and gel time of a silicon source, and the reaction time of the mixed acid on the gel is only 1 hour in the embodiment, so that compared with the comparative example (hydrolysis of 3 hours+gel of 6-8 hours) using sulfuric acid, the reaction efficiency is greatly improved; (2) The addition of the flame retardant effectively improves the limiting oxygen index of the silica aerogel and improves the flame retardant property of the silica aerogel.
Application example 1
The application of the flame-retardant silica aerogel in the fireproof paint comprises the following steps:
Table 1 fireproof paint formulation (mass fraction)
The raw materials were weighed first according to the formulation of table 1. Adding water, a fireproof auxiliary agent (APP, MEL, PER), titanium dioxide, a proper amount of auxiliary agent and the like into a container, stirring, mixing, grinding to required fineness by three rollers, adding emulsion and a curing agent, uniformly mixing to obtain a common fireproof heat-insulating coating A, respectively adding a common silica aerogel and a flame-retardant silica aerogel (example 3) on the basis of the formula of the common fireproof heat-insulating coating A, replacing titanium dioxide with corresponding weight, and slightly stirring to be uniform to obtain a silica fireproof heat-insulating coating B and a flame-retardant silica fireproof heat-insulating coating C.
Combustion performance test:
And (3) polishing and derusting the steel plate (150mm x 70mm x 1mm) by using sand paper, then brushing various fireproof coatings obtained by the preparation, naturally airing, and brushing again after 24 hours until the thickness of the coating reaches 2+/-0.1 mm. The sample plate is placed at the position 10cm above the gas lamp for burning for 60min, the temperature of the back surface of the steel plate is measured, and after the test is finished, the thickness of the charring layer of the fire-receiving point is measured by a vernier caliper, and the ratio of the expansion thickness to the original thickness of the coating is the foaming multiplying power of the fireproof coating.
TABLE 2
As can be seen from the table, the heat insulation and flame retardance of the coating are obviously improved after the silica aerogel is added, and compared with the common silica aerogel, the heat insulation and flame retardance of the flame-retardant silica aerogel provided by the invention are further improved, because the heat stability of the silica aerogel is improved by adding the flame retardant, the flame retardant can release flame retardant gas during thermal decomposition, the cell structure of an expansion layer of the coating is improved, and the fireproof and heat insulation performance of the coating is further improved.
The applicant states that the detailed process flow of the present invention is illustrated by the above examples, but the present invention is not limited to the above detailed process flow, i.e. it does not mean that the present invention must be implemented depending on the above detailed process flow. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.
Claims (6)
1. A preparation method of flame-retardant silica aerogel is characterized by comprising the following steps: the method comprises the following steps:
(1) Uniformly mixing water glass and water at room temperature, adding hexamethyldisilazane and n-hexane, and uniformly stirring to obtain a mixed solution;
(2) Adding an inorganic acid catalyst and a flame retardant into the mixed solution, uniformly stirring, adding ammonia water to adjust the pH to be 8-9, standing for 0.5-2 h at room temperature, and removing a water layer after layering the solution to obtain a silica wet gel;
The inorganic acid catalyst is a mixture of phosphoric acid and hydrofluoric acid, the mass ratio of the phosphoric acid to the hydrofluoric acid is 1-3:1, the inorganic acid catalyst accounts for 2-10% of the total mass of the mixed solution, and the flame retardant accounts for 0.5-1.5% of the total mass of the mixed solution;
the flame retardant is ammonium polyphosphate;
(3) Aging the silica wet gel at room temperature for at least 24 h, and respectively performing solvent replacement in ethanol and n-hexane;
(4) Drying the silica wet gel subjected to solvent replacement at normal pressure to obtain the flame-retardant silica aerogel;
The solvent replacement method is to soak the silica wet gel in a corresponding solvent at room temperature for 24-72 h.
2. The method for preparing the flame-retardant silica aerogel according to claim 1, wherein: the mass ratio of the water glass to the water to the hexamethyldisilazane to the n-hexane in the mixed solution is 1:3-5:0.2-2:3-15.
3. The method for preparing the flame-retardant silica aerogel according to claim 1, wherein: the normal pressure drying treatment method comprises the following steps: and respectively drying the silica wet gel subjected to solvent replacement at 50 ℃,80 ℃, 110 ℃, 150 ℃ and 180 ℃ for 2-6 hours under normal pressure, and naturally cooling to 25 ℃.
4. A flame retardant silica aerogel characterized by: which is obtainable by the process according to any one of claims 1 to 3.
5. The flame retardant silica aerogel of claim 4 wherein: the heat conductivity coefficient is 0.02-0.05W/mK, the water contact angle is more than 120 degrees, and the oxygen index is more than or equal to 28.
6. The use of the flame retardant silica aerogel according to claim 4 in fire retardant coatings.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104231798A (en) * | 2013-06-19 | 2014-12-24 | 河南工业大学 | Modified silicon dioxide aerogel microsphere thermal-insulation coating |
| CN112624129A (en) * | 2020-12-23 | 2021-04-09 | 上海应用技术大学 | Method for preparing silicon dioxide aerogel material by continuous heating method |
| CN113683387A (en) * | 2020-05-18 | 2021-11-23 | 江苏泛亚微透科技股份有限公司 | Hydrophobic flame-retardant silicon dioxide aerogel ceramic fiber felt and preparation method thereof |
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