CN113185149A - Fireproof glass and preparation method thereof - Google Patents

Fireproof glass and preparation method thereof Download PDF

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Publication number
CN113185149A
CN113185149A CN202110637903.0A CN202110637903A CN113185149A CN 113185149 A CN113185149 A CN 113185149A CN 202110637903 A CN202110637903 A CN 202110637903A CN 113185149 A CN113185149 A CN 113185149A
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temperature
glass
curing
agent
fireproof
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李冬威
刘郁
崔洪伟
白福臣
聂伟
庄婷婷
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Changchun Institute of Applied Chemistry of CAS
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Changchun Institute of Applied Chemistry of CAS
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
    • C03C27/06—Joining glass to glass by processes other than fusing
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
    • C03C27/06—Joining glass to glass by processes other than fusing
    • C03C27/10—Joining glass to glass by processes other than fusing with the aid of adhesive specially adapted for that purpose
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K21/00—Fireproofing materials
    • C09K21/02—Inorganic materials

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Inorganic Chemistry (AREA)
  • Joining Of Glass To Other Materials (AREA)

Abstract

The invention provides a preparation method of microbubble-free low-temperature-resistant perfusion type fireproof glass, which comprises the following steps: adding condensing agent, defoaming agent, antioxidant, light stabilizer, flatting agent and other assistants into silica sol, mixing, adding curing agent, defoaming and obtaining fireproof liquid; and pouring the fire-proof liquid into the laminated glass for curing to obtain the pouring type fire-proof glass. According to the invention, through formula development, the high-efficiency condensing agent is obtained by compounding specific raw materials according to a certain proportion, the light transmittance of the prepared pouring type fireproof glass can reach 87.4%, the light transmittance change after 100h of radiation irradiation resistance is less than 3.5%, the glass is basically bubble-free, the fire resistance and heat insulation can reach 90min, the glass does not freeze for a long time at the temperature of minus 20 +/-2 ℃, the defects that the pouring type fireproof glass is easy to freeze and the light transmittance is reduced due to low-temperature fireproof liquid are effectively overcome, and the market application prospect of the pouring type fireproof glass in a low-temperature environment is widened. The invention also provides the fireproof glass.

Description

Fireproof glass and preparation method thereof
Technical Field
The invention belongs to the technical field of glass, and particularly relates to fireproof glass and a preparation method thereof.
Background
The fireproof glass is functional glass, has good transmittance, can block and weaken smoke, flame and heat radiation, and has the functions of controlling fire spread, isolating smoke, insulating heat and the like. According to the definition in GB/T15763.1-2001 'safety glass for building' fire-proof glass, the fire-proof glass is mainly divided into single-piece fire-proof glass (DFB) and composite fire-proof glass (FFB), but the application range of the single-piece fire-proof glass is limited because the single-piece fire-proof glass has no heat insulation property, the composite fire-proof glass is formed by compounding two or more layers of glass and a thermal expansion material, the glass is rapidly exploded after being heated, and the thermal expansion material expands to about ten times after absorbing heat, so that the fire-proof and heat-insulation effects can be effectively achieved. According to different processes, the composite fireproof glass can be divided into a pouring type and a sandwich type, wherein the pouring type fireproof glass is formed by sealing the periphery of two or more layers of plate glass through a special sealing flame-retardant adhesive tape, then injecting fireproof liquid into a cavity between glass sheets through a preset pouring opening, solidifying the fireproof liquid to form a transparent colloidal substance, bonding the two layers of glass together, and finally sealing to form a fireproof glass component.
The fireproof glass in the prior art generally has the problems that the transmittance is low, and the transmittance is influenced by icing and whitening in a low-temperature environment.
Disclosure of Invention
In view of the above, the present invention provides a fire-proof glass and a preparation method thereof, and the fire-proof glass prepared by the method provided by the present invention is not easy to generate ice flowers and ice in a low temperature environment.
The invention provides a preparation method of fireproof glass, which comprises the following steps:
1) mixing silica sol, a defoaming agent, an antioxidant, a light stabilizer, a flatting agent and a condensing agent to obtain silica sol dispersion liquid;
2) mixing the silica sol dispersion liquid and a curing agent, and removing bubbles to obtain low-temperature-resistant fireproof liquid;
3) pouring the low-temperature-resistant fireproof liquid into a cavity of the sandwich hollow glass, and then curing to obtain fireproof glass;
the condensing agent comprises: ethylene glycol, ethanol, glycerol and Na2HPO4Sodium fatty alcohol-polyoxyethylene ether sulfate, coconut oil fatty acid diethanolamide and alkylphenol polyoxyethylene.
Preferably, the glycol, ethanol, glycerol and Na2HPO4The mass ratio of the fatty alcohol-polyoxyethylene ether sodium sulfate to the coconut oil fatty acid diethanolamide to the alkylphenol ethoxylates is (35-55): (35-45): (5-20): (1-2): (0.2-1.5): (0.2-0.5): (0.2-0.5).
Preferably, the silica sol is selected from the group consisting of alkaline silica sols;
the defoaming agent is selected from one or more of cardanol polyoxyethylene ether;
the antioxidant is selected from one or two of isoascorbic acid and L-ascorbic acid;
the light stabilizer is selected from bis (1-octyloxy-2, 2,6, 6-tetramethyl-4-piperidyl) sebacate;
the leveling agent is selected from one or more of polyether modified organic silicon;
the curing agent is selected from potassium hydroxide aqueous solution.
Preferably, the mass ratio of the silica sol to the defoaming agent to the antioxidant to the light stabilizer to the leveling agent to the condensing agent to the curing agent is (55-70): (0.2-1): (0.5-2): (0.2-1): (0.2-1): (8-12): (15-30).
Preferably, the molar ratio of the silicon dioxide in the silica sol to the potassium hydroxide in the curing agent is (2-2.5): 1.
preferably, the mixing temperature in the step 1) is 30-50 ℃.
Preferably, the mixing temperature in the step 2) is 30-50 ℃.
Preferably, the method for removing bubbles is vacuuming and removing bubbles.
Preferably, the curing method in step 3) comprises:
after the poured product is subjected to first curing, sealing a grouting opening and then performing second curing to obtain fireproof glass;
the temperature of the first curing is 50-70 ℃;
the temperature of the second curing is 70-90 ℃.
The invention provides the fireproof glass prepared by the method in the technical scheme.
According to the invention, the efficient condensing agent is obtained by adopting specific raw materials and a proportion, and a curing mode of stepped temperature rise and pressure rise is adopted in the process of preparing the fireproof glass, so that the microbubble-free low-temperature-resistant fireproof glass is obtained, the problems of ice flowers and icing of the fireproof glass in a long-term low-temperature environment are effectively solved, and the application and popularization of the fireproof glass in a low-temperature area can be widened.
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 preparation method of fireproof glass, which comprises the following steps:
1) mixing silica sol, a defoaming agent, an antioxidant, a light stabilizer, a flatting agent and a condensing agent to obtain silica sol dispersion liquid;
2) mixing the silica sol dispersion liquid and a curing agent, and removing bubbles to obtain low-temperature-resistant fireproof liquid;
3) pouring the low-temperature-resistant fireproof liquid into a cavity of the sandwich hollow glass, and then curing to obtain fireproof glass;
the condensing agent comprises: ethylene glycol, ethanol, glycerol and Na2HPO4Sodium fatty alcohol-polyoxyethylene ether sulfate, coconut oil fatty acid diethanolamide and alkylphenol polyoxyethylene.
In the invention, the silica sol is preferably alkaline silica sol, the solid content of the silica sol is preferably 40-50%, more preferably 50%, and the silica sol has better fire resistance; the particle size of the silica sol is preferably 90-110 nm, more preferably 95-105 nm, and most preferably 100 nm.
In the invention, the defoaming agent is preferably selected from one or more of cardanol polyoxyethylene ether, more preferably selected from one or more of cardanol polyoxyethylene ether BGF-6, cardanol polyoxyethylene ether BGF-7, cardanol polyoxyethylene ether BGF-9 and cardanol polyoxyethylene ether BGF-10.
In the present invention, the antioxidant is preferably selected from one or two of erythorbic acid and L-ascorbic acid.
In the present invention, the light stabilizer is preferably selected from bis (1-octyloxy-2, 2,6, 6-tetramethyl-4-piperidyl) sebacate, such as BSF UV-123 product.
In the invention, the leveling agent is preferably selected from one or more polyether modified organic silicon, and more preferably one or two of BYK-301 and BYK-333.
In the present invention, the condensing agent includes:
ethylene glycol, ethanol, glycerol and Na2HPO4Sodium fatty alcohol-polyoxyethylene ether sulfate, coconut oil fatty acid diethanolamide and alkylphenol polyoxyethylene.
In the invention, the glycol, the ethanol, the glycerol and the Na2HPO4The mass ratio of the fatty alcohol-polyoxyethylene ether sodium sulfate to the coconut oil fatty acid diethanolamide to the alkylphenol ethoxylates is preferably (35-55): (35-45): (5-20): (1-2): (0.2-1.5): (0.2-0.5): (0.2 to 0.5), more preferably (40 to 50): (37-40): (8-15): (1.5-2): (0.3-1.0): (0.2-0.4): (0.2 to 0.4), more preferably (45 to 50): (37-38): (9-12): (1.8-2): (0.5-0.8): (0.2-0.3): (0.2 to 0.3), most preferably 50: 37: 10: 2: 0.6: 0.2: 0.2.
in the present invention, the method for preparing the condensing agent preferably includes:
mixing ethylene glycol, ethanol, glycerol, and Na2HPO4Mixing the sodium alcohol ether sulphate, the cocoanut oil fatty acid diethanolamide and the alkylphenol ethoxylates to obtain the condensing agent.
In the invention, the mixing is preferably carried out under the condition of stirring, and the stirring time is preferably 15-25 min, more preferably 18-22 min, and most preferably 20 min; the mixing temperature is preferably normal temperature, more preferably 20-30 ℃, more preferably 22-28 ℃, more preferably 24-26 ℃, and most preferably 25 ℃.
In the invention, the mass ratio of the silica sol, the defoaming agent, the antioxidant, the light stabilizer, the flatting agent, the condensing agent and the curing agent is preferably (55-70): (0.2-1): (0.5-2): (0.2-1): (0.2-1): (8-12): (15-30), more preferably (60-65): (0.5-1): (0.5-1): (0.5-1): (0.5-1): (10-12): (20-25), more preferably (61-63): (0.8-1): (0.5-0.8): (0.8-1): (0.5-0.8): (11-12): (22-24), most preferably 62: 1: 0.5: 1: 0.5: 12: 23.
in the present invention, SiO in the silica sol2And the molar ratio of KOH in the curing agent is preferably (2-2.5): 1, more preferably (2.1 to 2.4): 1, most preferably (2.2-2.3): 1, in the range, the light transmittance of the prepared microbubble-free low-temperature perfusion-resistant fireproof glass is 87.4 percent, the light transmittance changes by less than 3.5 percent after 100 hours of radiation irradiation resistance, the microbubble is basically avoided, the fireproof and heat-insulating properties can reach 90min (the thickness of two cavities of the glass is 17cm in total, and the thickness of a fireproof cavity is 6cm in total), and the microbubble-free low-temperature perfusion-resistant fireproof glass does not freeze and whiten for a long time at the temperature of 20 +/-2 ℃.
In the invention, the mixing temperature in the step 1) is preferably 30-50 ℃, more preferably 35-45 ℃, and most preferably 40 ℃.
In the present invention, the method for mixing in step 1) preferably includes:
and at room temperature, stirring the silica sol, the defoaming agent, the antioxidant, the light stabilizer and the flatting agent, adding the condensing agent, heating and then continuing stirring to obtain the silica sol dispersion liquid.
In the invention, the temperature of the room temperature is consistent with the normal temperature in the technical scheme, and is not described again; the stirring time is preferably 5-15 min, more preferably 8-12 min, and most preferably 10 min; the temperature of the temperature rise is consistent with the temperature of the mixture in the step 1) of the technical scheme, and is not described again; the time for continuing stirring is preferably 25-35 min, more preferably 28-32 min, and most preferably 30 min.
In the invention, the curing agent is preferably a potassium hydroxide solution, more preferably a potassium hydroxide aqueous solution, and the mass concentration of the potassium hydroxide aqueous solution is preferably 40-60%, more preferably 45-55%, and most preferably 50%.
In the invention, the mixing temperature in the step 2) is preferably 35-45 ℃, more preferably 38-42 ℃, and most preferably 40 ℃.
In the present invention, the method for mixing in the step 2) preferably includes:
and slowly adding a curing agent into the silica sol dispersion liquid at the temperature of 30-50 ℃, wherein the system becomes turbid, and continuously stirring after all the curing agent is added until the system becomes clear from turbidity.
In the invention, the time for continuing stirring is preferably 25-35 min, more preferably 28-32 min, and most preferably 30 min.
In the invention, the method for removing bubbles is preferably vacuumized to remove bubbles; the vacuumizing pressure is preferably 0.05-0.15 MPa, more preferably 0.08-0.12 MPa, and most preferably 0.1 MPa; the time for vacuumizing and removing bubbles is preferably 0.5-1.5 hours, more preferably 0.8-1.2 hours, and most preferably 1 hour.
In the present invention, it is preferable that the defoaming further includes:
and cooling the product after defoaming to room temperature, and filtering to obtain the low-temperature-resistant fireproof liquid.
In the invention, the temperature of the room temperature is consistent with the temperature of the room temperature in the technical scheme, and is not described herein again; the filtration is preferably screen filtration; the aperture of the screen is preferably 150-250 meshes, more preferably 180-220 meshes, and most preferably 200 meshes.
In the present invention, the perfusion is preferably slow perfusion; the perfusion preferably further comprises:
and filling the cavity of the sandwich hollow glass with the low-temperature-resistant fireproof liquid, and then vibrating to remove bubbles.
The interlayer hollow glass is not particularly limited, and can be five-glass three-cavity hollow glass, three-glass two-cavity hollow glass or two-glass one-cavity hollow glass.
In the invention, the oscillation defoaming is preferably carried out in an ultrasonic cleaning instrument; the oscillation defoaming time is preferably 25-35 min, more preferably 28-32 min, and most preferably 30 min.
In the present invention, the method of curing preferably comprises:
and (5) carrying out first curing on the product subjected to the vibration and bubble removal, then sealing the grouting opening, and carrying out second curing to obtain the fireproof glass.
In the present invention, the curing is preferably performed in a vacuum oven, i.e., the first curing and the second curing are preferably performed in a vacuum oven.
In the invention, the temperature of the first curing is preferably 50-70 ℃, more preferably 55-65 ℃, and most preferably 60 ℃; the first curing is preferably carried out under negative pressure, and the pressure of the first curing is preferably 0.05-0.15 MPa, more preferably 0.08-0.12 MPa, and most preferably 0.1 MPa; the first curing time is preferably 2 to 6 hours, more preferably 3 to 5 hours, and most preferably 4 hours.
In the present invention, it is preferable to close the tank opening with a silicone sealant.
In the invention, the temperature of the second curing is preferably 70-90 ℃, more preferably 75-85 ℃, and most preferably 90 ℃; the second curing time is preferably 6 to 10 hours, more preferably 7 to 9 hours, and most preferably 8 hours.
According to the invention, the microbubble-free low-temperature-resistant pouring type glass fireproof liquid is prepared by adding the high-efficiency condensing agent prepared according to specific components and proportions and adopting a solidification mode of stepped temperature rise and pressure rise, so that the problems of ice flowers and icing of the fireproof glass in a long-term low-temperature environment are effectively solved, and the application and popularization of the fireproof glass in a low-temperature area can be widened.
The raw materials used in the following examples of the present invention are all commercially available products.
Example 1
50 parts by weight of ethylene glycol, 37 parts by weight of ethanol, 10 parts by weight of glycerol and 2 parts by weight of Na2HPO40.6 part by weight of sodium fatty alcohol polyoxyethylene ether sulfate (AES), 0.2 part by weight of coconut oil fatty acid diethanolamide (6501) and 0.2 part by weight of alkylphenol polyoxyethylene ether (TX-10), and stirring for 20min at normal temperature and uniformly mixing to obtain the condensing agent.
At room temperature, 62 parts by weight of 50% alkaline silica sol, 1 part by weight of defoaming agent (BGF-6), 0.5 part by weight of antioxidant erythorbic acid, 1 part by weight of light stabilizer (UV-123) and 0.5 part by weight of leveling agent (BYK-333) are put into a stirring container, stirring is started for 10min, then 12 parts by weight of the high-efficiency condensing agent are added, the temperature of the system is raised to 40 ℃, and stirring is carried out for 30min, so as to obtain stable and clear silica sol dispersion liquid.
At the temperature of 40 ℃, slowly adding 23 parts by weight of curing agent (50% KOH aqueous solution by mass concentration) into the silica sol dispersion, wherein the system becomes turbid, continuously stirring for 30min after all the curing agent is added until the system becomes clear from turbid, vacuumizing and removing bubbles for 1h under the pressure of 0.1MPa, then cooling to room temperature, and filtering by using a 200-mesh screen to obtain the low-temperature-resistant fireproof liquid.
Slowly pouring the low-temperature-resistant fireproof liquid into a cavity (three-glass two-cavity) of the interlayer hollow glass, placing the interlayer hollow glass into an ultrasonic cleaner to shake and remove bubbles for 30min after the cavity is filled with the fireproof liquid, then placing the interlayer hollow glass into a vacuum oven, curing for 4h at the negative pressure of 0.1MPa at the temperature of 60 ℃, taking out the interlayer hollow glass, sealing a grouting opening with silicone sealant, and continuing curing for 8h at the temperature of 80 ℃ to obtain the microbubble-free low-temperature-resistant pouring type fireproof glass.
Example 2
50 parts by weight of ethylene glycol, 37 parts by weight of ethanol, 10 parts by weight of glycerol and 2 parts by weight of Na2HPO40.6 weight part of fatty alcohol-polyoxyethylene ether sodium sulfate (AES) and 0.2 weight part of coconut oil fatty acidDiethanolamide (6501) and 0.2 part by weight of alkylphenol polyoxyethylene (TX-10), and stirring at normal temperature for 20min to obtain the condensing agent.
At room temperature, 58 parts by weight of 50% alkaline silica sol, 1 part by weight of defoaming agent (BGF-333), 0.5 part by weight of antioxidant (L-ascorbic acid), 1 part by weight of light stabilizer (UV-123) and 0.5 part by weight of leveling agent (BYK-301) are placed into a stirring container, stirring is started for 10min, then 12 parts by weight of the prepared high-efficiency condensing agent is added, the system temperature is raised to 40 ℃, and stirring is carried out for 30min, so as to obtain stable and clear silica sol dispersion liquid.
At the temperature of 40 ℃, slowly adding 27 parts by weight of a curing agent (KOH aqueous solution with the mass concentration of 50%) into the prepared silica sol dispersion liquid, wherein the system becomes turbid, continuously stirring for 30min after all the curing agent is added until the system becomes clear from the turbidity, vacuumizing and removing bubbles for 1h under the pressure of 0.1MPa, then cooling to room temperature, and filtering with a 200-mesh screen to obtain the low-temperature-resistant fireproof liquid.
Slowly pouring the low-temperature-resistant fireproof liquid into a cavity (three-glass two-cavity) of the interlayer hollow glass, placing the interlayer hollow glass into an ultrasonic cleaner to shake and remove bubbles for 30min after the cavity is filled with the glass liquid, then placing the interlayer hollow glass into a vacuum oven, curing for 4h at the negative pressure of 0.1MPa at the temperature of 60 ℃, taking out the interlayer hollow glass, sealing a grouting opening with silicone sealant, and continuing curing for 8h at the temperature of 80 ℃ to obtain the microbubble-free low-temperature-resistant pouring type fireproof glass.
Example 3
Mixing 40 parts by weight of ethylene glycol, 37 parts by weight of ethanol, 10 parts by weight of glycerol and 2 parts by weight of Na2HPO40.6 part by weight of sodium fatty alcohol polyoxyethylene ether sulfate (AES), 0.2 part by weight of coconut oil fatty acid diethanolamide (6501) and 0.2 part by weight of alkylphenol polyoxyethylene ether (TX-10), and stirring for 20min at normal temperature and uniformly mixing to obtain the condensing agent.
At room temperature, 65 parts by weight of 40% alkaline silica sol, 1 part by weight of defoaming agent (BGF-07), 0.5 part by weight of antioxidant L-ascorbic acid, 1 part by weight of light stabilizer (UV-123) and 0.5 part by weight of leveling agent (BYK-301) are placed into a stirring container, stirring is started for 10min, 12 parts by weight of the prepared efficient condensing agent is added, then the temperature of the system is raised to 40 ℃, and stirring is carried out for 30min, so as to obtain stable and clear silica sol dispersion liquid.
At the temperature of 40 ℃, 20 parts by weight of curing agent (50% KOH aqueous solution by mass concentration) is slowly added into the prepared silica sol dispersion liquid, the system becomes turbid, the stirring is continued for 30min after all the curing agent is added until the system becomes clear from the turbidity, then the vacuumizing is carried out for bubble removal for 1h under the pressure of 0.1MPa, then the temperature is reduced to the room temperature, and the low-temperature resistant fireproof liquid is obtained after the filtering by a 200-mesh screen.
Slowly pouring the prepared low-temperature-resistant fireproof liquid into a cavity (three-glass two-cavity) of the laminated hollow glass, placing the laminated hollow glass into an ultrasonic cleaner to shake and remove bubbles for 30min after the cavity is filled with the low-temperature-resistant fireproof liquid, then placing the laminated hollow glass into a vacuum oven, curing for 4h at the temperature of 60 ℃ and the negative pressure of 0.1MPa, taking out the laminated hollow glass, sealing a grouting opening with silicone sealant, and continuously curing for 8h at the temperature of 80 ℃ to obtain the microbubble-free low-temperature-resistant pouring type fireproof glass.
Example 4
50 parts by weight of ethylene glycol, 37 parts by weight of ethanol, 10 parts by weight of glycerol and 2 parts by weight of Na2HPO40.6 part by weight of sodium Alcohol Ether Sulphate (AES), 0.2 part by weight of coconut oil fatty acid diethanolamide (6501) and 0.2 part by weight of alkylphenol polyoxyethylene (TX-10) are stirred and mixed evenly at normal temperature for 20min to obtain the condensing agent.
At room temperature, 65 weight parts of 50% alkaline silica sol, 1 weight part of defoaming agent (BGF-10), 0.5 weight part of antioxidant erythorbic acid, 1 weight part of light stabilizer (UV-123) and 0.5 weight part of flatting agent (BYK-333) are put into a stirring container, after stirring for 10min, 8 weight parts of the prepared high-efficiency condensing agent is added, then the temperature of the system is raised to 40 ℃, and stirring is carried out for 30min, so as to obtain stable and clear silica sol dispersion liquid.
Slowly adding 24 parts by weight of curing agent (50% KOH aqueous solution by mass concentration) into the prepared silica sol dispersion liquid at 40 ℃, wherein the system becomes turbid, continuously stirring for 30min after all the curing agent is added until the system becomes clear from turbidity, vacuumizing and removing bubbles for 1h under 0.1MPa, then cooling to room temperature, and filtering by using a 200-mesh screen to obtain the low-temperature-resistant fireproof liquid.
Slowly pouring the prepared low-temperature-resistant fireproof liquid into a cavity (three-glass two-cavity) of the laminated hollow glass, placing the laminated hollow glass into an ultrasonic cleaner to shake and remove bubbles for 30min after the cavity is filled with the low-temperature-resistant fireproof liquid, then placing the laminated hollow glass into a vacuum oven, curing for 4h at the temperature of 60 ℃ and the negative pressure of 0.1MPa, taking out the laminated hollow glass, sealing a grouting opening with silicone sealant, and continuously curing for 8h at the temperature of 80 ℃ to obtain the microbubble-free low-temperature-resistant pouring type fireproof glass.
Example 5
Mixing 40 parts by weight of ethylene glycol, 45 parts by weight of ethanol, 15 parts by weight of glycerol and 2 parts by weight of Na2HPO40.6 part by weight of sodium Alcohol Ether Sulphate (AES), 0.2 part by weight of coconut oil fatty acid diethanolamide (6501) and 0.2 part by weight of alkylphenol polyoxyethylene (TX-10) are stirred and mixed evenly at normal temperature for 20min to obtain the condensing agent.
At room temperature, 65 weight parts of 50% alkaline silica sol, 1 weight part of defoaming agent (BGF-9), 0.5 weight part of antioxidant (isoascorbic acid), 1 weight part of light stabilizer (UV-123) and 0.5 weight part of flatting agent (BYK-301) are put into a stirring container, after stirring for 10min, 12 weight parts of the prepared high-efficiency condensing agent is added, then the temperature of the system is raised to 40 ℃, and stirring is carried out for 30min, so as to obtain stable and clear silica sol dispersion liquid.
Slowly adding 24 parts by weight of curing agent (50% KOH aqueous solution by mass concentration) into the prepared silica sol dispersion liquid at 40 ℃, wherein the system becomes turbid, continuously stirring for 30min after all the curing agent is added until the system becomes clear from turbidity, vacuumizing and removing bubbles for 1h under 0.1MPa, then cooling to room temperature, and filtering by using a 200-mesh screen to obtain the low-temperature-resistant fireproof liquid.
Slowly pouring the prepared low-temperature-resistant fireproof liquid into a cavity (three-glass two-cavity) of the laminated hollow glass, placing the laminated hollow glass into an ultrasonic cleaner to shake and remove bubbles for 30min after the cavity is filled with the low-temperature-resistant fireproof liquid, then placing the laminated hollow glass into a vacuum oven, curing for 4h at the temperature of 60 ℃ and the negative pressure of 0.1MPa, taking out the laminated hollow glass, sealing a grouting opening with silicone sealant, and continuously curing for 8h at the temperature of 80 ℃ to obtain the microbubble-free low-temperature-resistant pouring type fireproof glass.
Performance detection
The total thickness of the fireproof glass prepared by the embodiment of the invention is 17cm, and the total thickness of the fireproof cavity is 6 cm. According to GB/T9978.1-2008' method for fire resistance test of building elements part 1: general requirements, GB/T12513-: the method of fire-proof glass, the appearance, light transmittance, ultraviolet resistance, fire resistance and heat insulation of the fire-proof glass prepared in the example, and the cold resistance (-20 ℃) are detected as follows:
Figure BDA0003105923060000091
Figure BDA0003105923060000101
according to the invention, the microbubble-free low-temperature-resistant pouring type glass fireproof liquid is prepared by adding the high-efficiency condensing agent prepared according to specific components and proportions and adopting a solidification mode of stepped temperature rise and pressure rise, so that the problems of ice flowers and icing of the fireproof glass in a long-term low-temperature environment are effectively solved, and the application and popularization of the fireproof glass in a low-temperature area can be widened.
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. A preparation method of fireproof glass comprises the following steps:
1) mixing silica sol, a defoaming agent, an antioxidant, a light stabilizer, a flatting agent and a condensing agent to obtain silica sol dispersion liquid;
2) mixing the silica sol dispersion liquid and a curing agent, and removing bubbles to obtain low-temperature-resistant fireproof liquid;
3) pouring the low-temperature-resistant fireproof liquid into a cavity of the sandwich hollow glass, and then curing to obtain fireproof glass;
the condensing agent comprises: ethylene glycol, ethanol, glycerol and Na2HPO4Sodium fatty alcohol-polyoxyethylene ether sulfate, coconut oil fatty acid diethanolamide and alkylphenol polyoxyethylene.
2. The method of claim 1, wherein the glycol, ethanol, glycerol, Na2HPO4The mass ratio of the fatty alcohol-polyoxyethylene ether sodium sulfate to the coconut oil fatty acid diethanolamide to the alkylphenol ethoxylates is (35-55): (35-45): (5-20): (1-2): (0.2-1.5): (0.2-0.5): (0.2-0.5).
3. The method according to claim 1, wherein the silica sol is selected from the group consisting of alkaline silica sols;
the defoaming agent is selected from one or more of cardanol polyoxyethylene ether;
the antioxidant is selected from one or two of isoascorbic acid and L-ascorbic acid;
the light stabilizer is selected from bis (1-octyloxy-2, 2,6, 6-tetramethyl-4-piperidyl) sebacate;
the leveling agent is selected from one or more of polyether modified organic silicon;
the curing agent is selected from potassium hydroxide aqueous solution.
4. The method according to claim 1, wherein the mass ratio of the silica sol to the defoaming agent to the antioxidant to the light stabilizer to the leveling agent to the curing agent is (55-70): (0.2-1): (0.5-2): (0.2-1): (0.2-1): (15-30).
5. The method according to claim 1, wherein the molar ratio of the silica in the silica sol to the potassium hydroxide in the curing agent is (2-2.5): 1.
6. the method according to claim 1, wherein the temperature for mixing in step 1) is 30 to 50 ℃.
7. The method according to claim 1, wherein the temperature for mixing in the step 2) is 30 to 50 ℃.
8. The method of claim 1, wherein the bubble removal method is vacuuming bubble removal.
9. The method of claim 1, wherein the curing in step 3) comprises:
after the poured product is subjected to first curing, sealing a grouting opening and then performing second curing to obtain fireproof glass;
the temperature of the first curing is 50-70 ℃;
the temperature of the second curing is 70-90 ℃.
10. A fire-resistant glass made by the method of claim 1.
CN202110637903.0A 2021-06-08 2021-06-08 Fireproof glass and preparation method thereof Pending CN113185149A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114956606A (en) * 2022-04-25 2022-08-30 江苏福坤新材料科技有限公司 Processing method of anti-collision heat-insulation fireproof glass and vacuum filling device thereof
CN115353298A (en) * 2022-09-20 2022-11-18 江苏铁锚玻璃股份有限公司 Low-temperature-resistant fireproof glass and preparation method thereof
CN115370272A (en) * 2022-09-20 2022-11-22 江苏铁锚玻璃股份有限公司 High-light-transmittance heat-insulation fireproof glass and preparation method thereof

Citations (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0557068A1 (en) * 1992-02-18 1993-08-25 Pilkington Plc Curing epoxy resins
CN1110666A (en) * 1995-03-09 1995-10-25 公安部天津消防科学研究所 Fireproof glass
JPH0911412A (en) * 1995-04-28 1997-01-14 Toray Ind Inc Laminated moldings
JP2002316841A (en) * 2001-04-19 2002-10-31 Central Glass Co Ltd Method for manufacturing hydrous gel fire preventive glass and apparatus for manufacturing the same
WO2008154994A1 (en) * 2007-06-16 2008-12-24 Scheuten Glasgroep B.V. Method for producing a fire protection agent
CN104072056A (en) * 2014-05-23 2014-10-01 安徽阜阳思科达科技建材有限公司 Fireproof thermal mortar
CN105131872A (en) * 2015-09-07 2015-12-09 中国建筑材料科学研究总院 Fireproof liquid of composite fireproof glass and preparation method thereof and composite fireproof glass
CN106883797A (en) * 2017-02-21 2017-06-23 中国建筑材料科学研究总院 A kind of fireproof gum liquid-based matter and preparation method thereof and fire prevention glue and preparation method thereof
CN107216638A (en) * 2017-07-12 2017-09-29 苏州珀力玛高分子材料有限公司 A kind of temperature becomes light modulation fire proofing material, temperature control sunshade flame resistant glass and preparation method thereof
CN107244129A (en) * 2017-06-22 2017-10-13 合肥钢骨玻璃制品有限公司 A kind of preparation method of composite fireproof glass
CN107267103A (en) * 2016-04-08 2017-10-20 卢斌 Transparent heat-insulated fireproof gum of a kind of aerogel-congtg and preparation method thereof and insulating fire-retarding glass
WO2018036426A1 (en) * 2016-08-22 2018-03-01 广东纳路纳米科技有限公司 Modified nanometer composite polysulfide sealant for fireproof glass and preparation method therefor
CN109095793A (en) * 2018-09-30 2018-12-28 江苏耀兴安全玻璃有限公司 A kind of preparation method of fireproof mezzanine glass
CN109679537A (en) * 2018-12-11 2019-04-26 中国建筑材料科学研究总院有限公司 Fire prevention layer material and preparation method thereof and flame resistant glass
CN109928650A (en) * 2017-12-15 2019-06-25 镇江兴谦新材料技术有限公司 A kind of preparation method of composite fireproof glass
CN209440837U (en) * 2019-01-25 2019-09-27 郑州福禄寿科技有限公司 It is used to prepare the penetration equipment of homogeneous fireproof heated board
CN110760206A (en) * 2019-10-29 2020-02-07 中国建筑材料科学研究总院有限公司 Fire-proof liquid and its preparation method
CN112662317A (en) * 2020-12-25 2021-04-16 中国建筑材料科学研究总院有限公司 Transparent fireproof glue, preparation method thereof and composite fireproof glass comprising transparent fireproof glue

Patent Citations (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0557068A1 (en) * 1992-02-18 1993-08-25 Pilkington Plc Curing epoxy resins
CN1110666A (en) * 1995-03-09 1995-10-25 公安部天津消防科学研究所 Fireproof glass
JPH0911412A (en) * 1995-04-28 1997-01-14 Toray Ind Inc Laminated moldings
JP2002316841A (en) * 2001-04-19 2002-10-31 Central Glass Co Ltd Method for manufacturing hydrous gel fire preventive glass and apparatus for manufacturing the same
WO2008154994A1 (en) * 2007-06-16 2008-12-24 Scheuten Glasgroep B.V. Method for producing a fire protection agent
CN104072056A (en) * 2014-05-23 2014-10-01 安徽阜阳思科达科技建材有限公司 Fireproof thermal mortar
CN105131872A (en) * 2015-09-07 2015-12-09 中国建筑材料科学研究总院 Fireproof liquid of composite fireproof glass and preparation method thereof and composite fireproof glass
CN107267103A (en) * 2016-04-08 2017-10-20 卢斌 Transparent heat-insulated fireproof gum of a kind of aerogel-congtg and preparation method thereof and insulating fire-retarding glass
WO2018036426A1 (en) * 2016-08-22 2018-03-01 广东纳路纳米科技有限公司 Modified nanometer composite polysulfide sealant for fireproof glass and preparation method therefor
CN106883797A (en) * 2017-02-21 2017-06-23 中国建筑材料科学研究总院 A kind of fireproof gum liquid-based matter and preparation method thereof and fire prevention glue and preparation method thereof
CN107244129A (en) * 2017-06-22 2017-10-13 合肥钢骨玻璃制品有限公司 A kind of preparation method of composite fireproof glass
CN107216638A (en) * 2017-07-12 2017-09-29 苏州珀力玛高分子材料有限公司 A kind of temperature becomes light modulation fire proofing material, temperature control sunshade flame resistant glass and preparation method thereof
CN109928650A (en) * 2017-12-15 2019-06-25 镇江兴谦新材料技术有限公司 A kind of preparation method of composite fireproof glass
CN109095793A (en) * 2018-09-30 2018-12-28 江苏耀兴安全玻璃有限公司 A kind of preparation method of fireproof mezzanine glass
CN109679537A (en) * 2018-12-11 2019-04-26 中国建筑材料科学研究总院有限公司 Fire prevention layer material and preparation method thereof and flame resistant glass
CN209440837U (en) * 2019-01-25 2019-09-27 郑州福禄寿科技有限公司 It is used to prepare the penetration equipment of homogeneous fireproof heated board
CN110760206A (en) * 2019-10-29 2020-02-07 中国建筑材料科学研究总院有限公司 Fire-proof liquid and its preparation method
CN112662317A (en) * 2020-12-25 2021-04-16 中国建筑材料科学研究总院有限公司 Transparent fireproof glue, preparation method thereof and composite fireproof glass comprising transparent fireproof glue

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
周春山主编: "《新编实用化工小商品产品规格及检验方法》", 31 December 1995, 中南工业大学出版社 *
宋启煌主编, 北京：化学工业出版社 *
廖文胜等编著: "《宾馆与家用洗涤剂配方设计》", 31 January 2000, 北京：中国轻工业出版社 *
朱洪法主编: "《生活化学品与健康》", 30 April 2013, 北京：金盾出版社 *
马贺伟等编著: "《皮革与纺织品环保指标及检测》", 31 July 2017, 北京：中国轻工业出版社 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114956606A (en) * 2022-04-25 2022-08-30 江苏福坤新材料科技有限公司 Processing method of anti-collision heat-insulation fireproof glass and vacuum filling device thereof
CN114956606B (en) * 2022-04-25 2023-08-22 江苏福坤新材料科技有限公司 Processing method of anti-collision heat-insulation fireproof glass and vacuum filling device thereof
CN115353298A (en) * 2022-09-20 2022-11-18 江苏铁锚玻璃股份有限公司 Low-temperature-resistant fireproof glass and preparation method thereof
CN115370272A (en) * 2022-09-20 2022-11-22 江苏铁锚玻璃股份有限公司 High-light-transmittance heat-insulation fireproof glass and preparation method thereof

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Application publication date: 20210730