Method for preparing composite fireproof glass through compatible tempered glass liquid lamination

Abstract

The invention relates to a method for preparing composite fireproof glass by laminating compatible tempered glass liquid. The method comprises the following steps: (1) spreading a fireproof liquid on at least one first glass substrate, and removing a solvent to form a cured film; (2) laminating the first glass substrate in a laminating liquid in a manner that the cured film faces upwards, covering the top surface with a second glass substrate, and laminating in the liquid to obtain a laminated sheet, wherein the laminated sheet is completely immersed in the laminating liquid; and (3) taking out the combined sheet, standing, aging, and carrying out post-treatment to obtain the composite fireproof glass. The prepared composite fireproof glass is excellent in hardness, light transmittance, low temperature resistance, irradiation resistance and the like, the whole glass layer is filled with gel, subsequent cutting and edging processes are not needed, and the composite fireproof glass can be compatible with tempered glass; the process is simple, expensive equipment and high-temperature, vacuum and other processes are not needed, and energy consumption is low.

Description

Technical Field

[0001] This invention relates to the field of fire-resistant glass preparation technology, and more particularly to a method for preparing composite fire-resistant glass by liquid lamination compatible with tempered glass. Background Technology

[0002] Composite fire-resistant glass is currently the only type of fire-resistant glass with heat insulation properties. Its basic structure consists of two or more layers of glass sandwiched with fire-resistant adhesive material. When exposed to high temperatures during a fire, the fire-resistant adhesive material rapidly foams and expands to form an insulating layer, effectively preventing the spread of fire and heat transfer. Composite fire-resistant glass not only possesses excellent heat insulation and fire resistance integrity (up to 3 hours), but also high light transmittance and good safety. With the continuous improvement of global building safety standards, the demand for composite fire-resistant glass is increasing, and it has a broad market prospect.

[0003] Composite fire-resistant glass is mainly classified into two types according to its production process: grouting and lamination. Grouting involves injecting fire-retardant liquid into a hollow interlayer composed of two or more layers of glass, and then solidifying the liquid at a certain temperature to form a fire-retardant gel. Grouting composite fire-resistant glass has a simple preparation process and high production efficiency. The technical difficulty lies in the formulation of the fire-retardant liquid. Taking the currently mainstream nano-silica sol fire-retardant liquids as an example (CN115353298A, CN114409279A, CN110305622A), precise control of the core-shell structure, particle size, dispersion, and solid content of silica nanoparticles is required through optimized formulation and process. This results in a more complex and costly preparation of the fire-retardant liquid. Furthermore, existing nano-silica composite fire-resistant glass generally has a high water content, leading to poor weather resistance, especially at low temperatures where it may exhibit whitening, freezing, and blistering, causing irreversible damage to the fire-retardant gel and affecting the appearance and function of the fire-resistant glass. At the same time, the high water content causes the gel layer to have certain rheological and swelling properties, which poses a potential safety hazard.

[0004] On the other hand, composite fire-resistant glass can also be prepared by lamination. The traditional lamination method involves spreading a mixture of silicate fire-retardant liquid or silicate particles and solution onto a glass plate. After drying some of the moisture (GB1590837A, GB2023452A), a gel is formed. Another glass plate is then pressed and bonded to the gel. High temperatures are required to soften the gel for easier lamination. During extrusion, numerous air bubbles exist between the gel and the glass plate, necessitating simultaneous vacuuming to remove them. Traditional lamination involves the simultaneous control of high temperature, high pressure, and vacuum, placing extremely high demands on equipment and manufacturing processes, resulting in high energy consumption and cost. However, the gel layer of composite fire-resistant glass prepared by lamination has extremely low water content (as low as 10%-20%), thus possessing advantages such as high bonding strength, no rheological properties, excellent light transmittance, and strong weather resistance. In particular, its low-temperature resistance can reach -50℃, making it popular in the high-end market.

[0005] Furthermore, for composite fire-resistant glass made from tempered glass, the industry typically employs a process of cutting before tempering to avoid damaging the edge strength of the tempered glass and causing it to shatter during cutting and grinding after tempering. However, existing lamination methods require further cutting of the original composite fire-resistant glass sheet after pressing to remove any remaining air bubbles and defects. Therefore, this type of process cannot use tempered glass and must use non-tempered glass. This makes this type of fire-resistant glass fragile during transportation and installation, and unsuitable for outdoor building applications requiring high strength.

[0006] While existing technologies such as grouting offer a simple process, the fire retardant liquid is expensive and the product has poor weather resistance. Traditional lamination methods, while producing high-performance products, require sophisticated equipment, resulting in high energy consumption and production costs, and cannot be used with tempered glass. Therefore, developing a composite fire-resistant glass manufacturing process that balances low cost, minimal equipment requirements, high weather resistance, high safety, and compatibility with tempered glass has become an urgent problem to be solved. Summary of the Invention

[0007] To address the aforementioned technical problems, this invention provides a method for preparing composite fireproof glass using liquid lamination compatible with tempered glass. This method eliminates the need for expensive lamination equipment and complex preparation processes, is simple to operate, significantly reduces energy consumption, and because the pressing process generates almost no bubbles, the gel fills the entire glass interlayer, eliminating the need for subsequent cutting and edge grinding processes. It is suitable for tempered glass.

[0008] To achieve this objective, the present invention adopts the following technical solution:

[0009] In a first aspect, the present invention provides a method for preparing composite fire-resistant glass using liquid lamination compatible with tempered glass, the method comprising the following steps:

[0010] (1) Fire retardant liquid is spread on at least one first glass substrate, and solvent is removed to form a cured film;

[0011] (2) The first glass substrate is stacked in the laminating liquid with the cured film facing upward, and the second glass substrate is covered on the top surface and then laminated underwater to obtain a laminate, wherein the laminating liquid completely immerses the laminate;

[0012] (3) After taking out the composite glass and letting it stand for aging, post-processing is carried out to obtain the composite fireproof glass.

[0013] The lamination of this invention is not carried out under conventional gas phase conditions, but in liquid phase. By placing the glass substrate containing the cured film and the glass cover plate entirely in the lamination liquid, air bubbles between the cured film layer and the glass can be completely eliminated. Then, by vertical extrusion, it can be pressed and shaped at room temperature.

[0014] The following are preferred technical solutions of the present invention, but are not intended to limit the technical solutions provided by the present invention. The purpose and beneficial effects of the present invention can be better achieved and realized through the following preferred technical solutions.

[0015] As a preferred technical solution of the present invention, the first glass substrate consists of 1 to 9 pieces, for example, 1, 2, 3, 4, 5, 6, 7, 8 or 9 pieces.

[0016] As a preferred embodiment of the present invention, the fire retardant liquid includes a silicate fire retardant liquid.

[0017] Preferably, the silicate fire retardant liquid comprises, by weight, 20-35 parts of silicate, for example, 20 parts, 25 parts, 30 parts, 33 parts, 35 parts, etc.; 2-15 parts of charring agent, for example, 2 parts, 5 parts, 8 parts, 12 parts, 15 parts, etc.; 1-5 parts of flame retardant, for example, 1 part, 2 parts, 3 parts, 4 parts, or 5 parts, etc.; 1-5 parts of refractory additive, for example, 1 part, 2 parts, 3 parts, 4 parts, or 5 parts, etc.; 0.3-1 part of defoamer, for example, 0.3 parts, 0.5 parts, 0.7 parts, 0.9 parts, or 1.0 part, etc.; and 50-80 parts of water, for example, 50 parts, 60 parts, 70 parts, 75 parts, or 80 parts, etc.

[0018] As a preferred embodiment of the present invention, the silicate is M2O·(SiO2). n M is a metallic element, which includes any one or a combination of at least two of sodium, potassium and lithium, and the modulus n of the silicate is 3-6, for example, it can be 3, 4, 5 or 6, etc.

[0019] Preferably, the char-forming agent includes any one or a combination of at least two of ethylene glycol, glycerol, sorbitol, pentaerythritol, sucrose, and fructose.

[0020] Preferably, the flame retardant comprises any one or a combination of at least two of ammonium polyphosphate, sodium polyphosphate, melamine phosphate, and water-soluble phosphate esters.

[0021] Preferably, the refractory additive includes any one or a combination of at least two of borax, urea and melamine.

[0022] Preferably, the defoamer comprises polyether-modified silicone.

[0023] As a preferred technical solution of the present invention, the water content of the cured film is 15-35wt%, for example, it can be 15wt%, 20wt%, 25wt%, 30wt% or 35wt%, etc.

[0024] This invention controls the moisture content of the cured film within the above-mentioned range so that the cured film has good surface wettability with the laminating liquid after being immersed in the laminating liquid. This further reduces the generation of microbubbles during the lamination process and avoids the decrease in weather resistance caused by excessive moisture content. As a result, the composite fireproof glass has good light transmittance, low temperature resistance and fire resistance.

[0025] Preferably, the thickness of the cured film is 0.5-3mm, for example, it can be 0.5mm, 1mm, 1.5mm, 2mm, 2.5mm or 3mm, etc.

[0026] The solvent removal method described in this invention includes, but is not limited to, natural air drying, which is sufficient to evaporate the solvent in the fire retardant liquid to a specific water content. Natural air drying refers to the natural evaporation of moisture in a clean space at room temperature. The time and temperature for solvent removal can be selected and optimized according to the water content requirements, and are not further limited here.

[0027] As a preferred technical solution of the present invention, the four edges of the first glass substrate are covered with water-resistant adhesive strips to maintain the thickness of the fireproof liquid, and the waterproof adhesive strips are removed after solvent removal.

[0028] As a preferred embodiment of the present invention, the laminating liquid comprises one or a combination of at least two of the following: pure water, ethanol, isopropanol, ethylene glycol, diethylene glycol, glycerol, and propylene glycol.

[0029] The laminating liquid selected in this invention has good surface wettability with the curing film. The bonding and lamination of the glass substrate are carried out by being completely immersed in the laminating liquid, which can effectively prevent the generation of microbubbles.

[0030] As a preferred technical solution of the present invention, the pressure of the submerged lamination is 1-10 MPa, for example, it can be 1 MPa, 3 MPa, 5 MPa, 8 MPa or 10 MPa, etc.

[0031] Preferably, the lamination holding time is 5-20 hours, for example, 5 hours, 8 hours, 10 hours, 15 hours or 20 hours.

[0032] The present invention preferably uses lamination pressure and time within the above range to ensure the interfacial adhesion between the cured film layer and the tempered glass, while avoiding damage to the tempered glass due to pressure overload. At the same time, it is compatible with conventional lamination equipment, requiring no additional upgrades and significantly reducing the process threshold.

[0033] The submersible lamination described in this invention can be performed using a manual or electric hydraulic press, as long as it can provide uniform pressure; no further limitations are imposed here.

[0034] As a preferred embodiment of the present invention, the first glass substrate and the second glass substrate are pretreated glass.

[0035] Preferably, the pretreatment includes cleaning to remove surface dirt and drying.

[0036] Preferably, the glass comprises tempered glass or float glass.

[0037] As a preferred technical solution of the present invention, the static aging time is 1-15 days, for example, it can be 1 day, 5 days, 10 days, 12 days or 15 days.

[0038] Preferably, the static aging process is carried out at room temperature.

[0039] Preferably, the post-processing includes removing the gel-like cured film that has been squeezed out from the edges.

[0040] This invention achieves a slow release of stress in the fire-retardant adhesive layer through static aging at room temperature, resulting in a more uniform and stable fire-retardant layer. The composite fire-retardant glass, after static aging, exhibits good light transmittance at the edges without microbubbles; only the extruded gel-like cured film needs to be removed, eliminating the need for cutting and edge grinding.

[0041] Compared with the prior art, the present invention has at least the following beneficial effects:

[0042] (1) The composite fireproof glass prepared by the present invention not only has excellent fire resistance, but also has excellent transparency, high bonding strength and excellent weather resistance. In particular, it can withstand low temperatures as low as -50℃ and can be widely used in various building scenarios such as fireproof doors and windows, partitions, and curtain walls.

[0043] (2) The preparation method provided by the present invention does not require cutting and post-processing, is compatible with tempered glass, does not rely on expensive equipment, and has a simple process and low energy consumption. Attached Figure Description

[0044] Figure 1(A) is a schematic flowchart of the method for preparing composite fireproof glass by liquid lamination of compatible tempered glass provided in Embodiments 1-13 of the present invention;

[0045] Figure 1 (B) is a schematic flowchart of the method for preparing composite fireproof glass by liquid lamination of compatible tempered glass provided in Embodiments 14-15 of the present invention. Detailed Implementation

[0046] To facilitate understanding of the present invention, the following embodiments are provided. Those skilled in the art should understand that these embodiments are merely illustrative and should not be construed as limiting the scope of the invention.

[0047] The glass substrates used in the following embodiments are all 110×60 cm in size.

[0048] Example 1

[0049] This embodiment provides a method for preparing composite fire-resistant glass using liquid-bed lamination compatible with tempered glass, the method comprising the following steps:

[0050] (1) Apply water-blocking adhesive strips to the edges of the cleaned and dried tempered glass plate, spread potassium silicate fire retardant liquid, and let it air dry naturally for 48 hours to form a cured film with a water content of 35% and a thickness of 2 mm. Then remove the water-blocking adhesive strips. The potassium silicate fire retardant liquid includes, by weight, 30 parts of potassium silicate (modulus 3.5), 5 parts of glycerin, 1 part of ammonium polyphosphate, 2 parts of borax, 0.3 parts of defoamer and 61.7 parts of water.

[0051] (2) Place the tempered glass plate with the cured film facing up in the laminating liquid, cover the top surface with a second tempered glass plate of the same size, and then laminate the sheets together using a press. The lamination pressure is 1 MPa, and the laminating liquid is ethanol and completely immerses the sheets together.

[0052] (3) After holding the pressure for 5 hours, release the pressure, take out the composite glass, let it stand at room temperature for 1 day, and then use a scraper to remove the gel-like cured film on the edge to obtain the composite fireproof glass with 2 glass and 1 adhesive.

[0053] Example 2

[0054] This embodiment provides a method for preparing composite fire-resistant glass using liquid-bed lamination compatible with tempered glass, the method comprising the following steps:

[0055] (1) Apply water-blocking adhesive strips to the edges of the cleaned and dried tempered glass plate, spread potassium silicate fire retardant liquid evenly, and let it air dry naturally for 48 hours to form a cured film with a water content of 30% and a thickness of 1.5 mm. Then remove the water-blocking adhesive strips. The potassium silicate fire retardant liquid includes, by weight, 28 parts of potassium silicate (modulus 3.7), 10 parts of glycerin, 1 part of ammonium polyphosphate, 2 parts of melamine, 0.3 parts of defoamer and 58.7 parts of water.

[0056] (2) Place the tempered glass plate with the cured film facing up in the laminating liquid, cover the top surface with a second tempered glass plate of the same size, and then laminate the sheets together using a press. The lamination pressure is 2 MPa, and the laminating liquid is isopropanol, which completely immerses the sheets.

[0057] (3) After holding the pressure for 5 hours, release the pressure, take out the composite glass and let it stand at room temperature for 2 days. Then use a scraper to remove the gel-like cured film on the edge to obtain the composite fireproof glass with 2 glass and 1 adhesive.

[0058] Example 3

[0059] This embodiment provides a method for preparing composite fire-resistant glass using liquid-bed lamination compatible with tempered glass, the method comprising the following steps:

[0060] (1) Apply water-blocking adhesive strips to the edges of the cleaned and dried tempered glass plate, spread potassium silicate fire retardant liquid, and let it air dry naturally for 48 hours to form a cured film with a water content of 35% and a thickness of 0.5mm. Then remove the water-blocking adhesive strips. The potassium silicate fire retardant liquid includes, by weight, 30 parts of potassium silicate (modulus 3.5), 5 parts of glycerin, 2 parts of ammonium polyphosphate, 3 parts of urea, 0.5 parts of defoamer and 59.5 parts of water.

[0061] (2) Place the tempered glass plate with the cured film facing up in the laminating liquid, cover the top surface with a second tempered glass plate of the same size, and then laminate the sheets together using a press. The lamination pressure is 1 MPa, and the laminating liquid is isopropanol, which completely immerses the sheets together.

[0062] (3) After holding the pressure for 5 hours, release the pressure, take out the composite glass, let it stand at room temperature for 5 days, and then use a scraper to remove the gel-like cured film on the edge to obtain the composite fireproof glass with 2 glass and 1 adhesive.

[0063] Example 4

[0064] This embodiment provides a method for preparing composite fire-resistant glass using liquid-bed lamination compatible with tempered glass, the method comprising the following steps:

[0065] (1) Apply water-blocking adhesive strips to the edges of the cleaned and dried tempered glass plate, spread potassium silicate fire retardant liquid, and let it air dry naturally for 48 hours to form a cured film with a water content of 33% and a thickness of 2.5 mm. Then remove the water-blocking adhesive strips. The potassium silicate fire retardant liquid includes, by weight, 25 parts of potassium silicate (modulus 4.0), 15 parts of glycerin, 1 part of sodium polyphosphate, 2 parts of urea, 0.3 parts of defoamer and 56.7 parts of water.

[0066] (2) The tempered glass plate is placed in the laminating liquid with the cured film facing up. After covering the top surface with a second tempered glass plate of the same size, the plates are laminated together using a press. The lamination pressure is 2 MPa, and the laminating liquid is ethylene glycol, which completely immerses the plates.

[0067] (3) After holding the pressure for 10 hours, release the pressure, take out the composite glass and let it stand at room temperature for 10 days. Then use a scraper to remove the gel-like cured film on the edge to obtain the composite fireproof glass with 2 glass and 1 adhesive.

[0068] Example 5

[0069] This embodiment provides a method for preparing composite fire-resistant glass using liquid lamination compatible with float glass, the method comprising the following steps:

[0070] (1) Apply water-blocking adhesive strips to the edges of the cleaned and dried float glass plate, spread potassium silicate fire retardant liquid evenly, and let it air dry naturally for 50 hours to form a cured film with a water content of 30% and a thickness of 2mm. Then remove the water-blocking adhesive strips. The potassium silicate fire retardant liquid includes, by weight, 30 parts of potassium silicate (modulus 3.5), 5 parts of sorbitol, 1 part of sodium polyphosphate, 2 parts of borax, 0.3 parts of defoamer and 61.7 parts of water.

[0071] (2) Place the float glass plate with the cured film facing up in the laminating liquid, cover the top surface with a second float glass plate of the same size, and then laminate the sheet using a press. The lamination pressure is 2 MPa, and the laminating liquid is ethanol and completely immerses the sheet.

[0072] (3) After holding the pressure for 15 hours, release the pressure, take out the composite glass and let it stand at room temperature for 15 days. Then use a scraper to remove the gel-like cured film on the edge to obtain the composite fireproof glass with 2 glass and 1 adhesive.

[0073] Example 6

[0074] This embodiment provides a method for preparing composite fire-resistant glass compatible with conventional float glass liquid lamination, the method comprising the following steps:

[0075] (1) Apply water-blocking adhesive strips to the edges of the cleaned and dried ordinary float glass plate, spread potassium silicate fire retardant liquid, and let it air dry naturally for 52 hours to form a cured film with a water content of 35% and a thickness of 3mm. Then remove the water-blocking adhesive strips. The potassium silicate fire retardant liquid includes, by weight, 30 parts of potassium silicate (modulus 3.5), 5 parts of sucrose, 1 part of ammonium polyphosphate, 2 parts of borax, 0.3 parts of defoamer and 61.7 parts of water.

[0076] (2) In the laminating liquid, a regular float glass plate is placed with the cured film facing upwards, and a second float glass plate of the same size is covered on the top surface. Then, the plates are laminated together using a press. The lamination pressure is 1 MPa, and the laminating liquid is isopropanol:water (1:1) and the plates are completely immersed in it.

[0077] (3) After holding the pressure for 5 hours, release the pressure, take out the composite glass and let it stand at room temperature for 10 days. Then use a scraper to remove the gel-like cured film on the edge to obtain the composite fireproof glass with 2 glass and 1 adhesive.

[0078] Example 7

[0079] This embodiment provides a method for preparing composite fire-resistant glass using liquid-bed lamination compatible with tempered glass, the method comprising the following steps:

[0080] (1) Apply water-blocking adhesive strips to the edges of the cleaned and dried tempered glass plate, spread potassium silicate fire retardant liquid evenly, and let it air dry naturally for 46 hours to form a cured film with a water content of 20% and a thickness of 1mm. Then remove the water-blocking adhesive strips. The potassium silicate fire retardant liquid includes, by weight, 25 parts potassium silicate (modulus 4.2), 5 parts glycerin, 1 part ammonium polyphosphate, 2 parts urea, 0.3 parts defoamer and 66.7 parts water.

[0081] (2) Place the tempered glass plate with the cured film facing up in the laminating liquid, cover the top surface with a second tempered glass plate of the same size, and then laminate the sheets together using a press. The lamination pressure is 10 MPa, and the laminating liquid is ethanol:water (1:1) and the sheets are completely submerged.

[0082] (3) After holding the pressure for 15 hours, release the pressure, take out the composite glass and let it stand at room temperature for 7 days. Then use a scraper to remove the gel-like cured film on the edge to obtain the composite fireproof glass with 2 glass and 1 adhesive.

[0083] Example 8

[0084] This embodiment provides a method for preparing composite fire-resistant glass using liquid-bed lamination compatible with tempered glass, the method comprising the following steps:

[0085] (1) Apply water-blocking adhesive strips to the edges of the cleaned and dried tempered glass plate, spread potassium silicate fire retardant liquid, and let it air dry naturally for 46 hours to form a cured film with a water content of 35% and a thickness of 2mm. Then remove the water-blocking adhesive strips. The potassium silicate fire retardant liquid includes, by weight, 25 parts potassium silicate (modulus 4.5), 5 parts ethylene glycol, 1 part ammonium polyphosphate, 2 parts borax, 0.3 parts defoamer and 66.7 parts water.

[0086] (2) The tempered glass plate is placed in the laminating liquid with the cured film facing up. After covering the top surface with a second tempered glass plate of the same size, the plates are laminated together using a press. The lamination pressure is 1 MPa, and the laminating liquid is propylene glycol, which completely immerses the plates.

[0087] (3) After holding the pressure for 5 hours, release the pressure, take out the composite glass, let it stand at room temperature for 1 day, and then use a scraper to remove the gel-like cured film on the edge to obtain the composite fireproof glass with 2 glass and 1 adhesive.

[0088] Example 9

[0089] This embodiment provides a method for preparing composite fire-resistant glass using liquid-bed lamination compatible with tempered glass, the method comprising the following steps:

[0090] (1) Apply water-blocking adhesive strips to the edges of the cleaned and dried tempered glass plate, spread sodium silicate fire retardant liquid, and let it air dry naturally for 50 hours to form a cured film with a water content of 15% and a thickness of 1.5 mm. Then remove the water-blocking adhesive strips. The sodium silicate fire retardant liquid includes, by weight, 30 parts sodium silicate (modulus 3.4), 5 parts glycerin, 1 part sodium polyphosphate, 2 parts borax, 0.3 parts defoamer and 61.7 parts water.

[0091] (2) The tempered glass plate is placed in the laminating liquid with the cured film facing up. After covering the top surface with a second tempered glass plate of the same size, the plates are laminated together using a press. The lamination pressure is 6 MPa, and the laminating liquid is ethanol, which completely immerses the plates.

[0092] (3) After holding the pressure for 12 hours, release the pressure, take out the composite glass, let it stand at room temperature for 6 days, and then use a scraper to remove the gel-like cured film on the edge to obtain the composite fireproof glass with 2 glass and 1 adhesive.

[0093] Example 10

[0094] This embodiment provides a method for preparing composite fire-resistant glass using liquid-bed lamination compatible with tempered glass, the method comprising the following steps:

[0095] (1) Apply water-blocking adhesive strips to the edges of the cleaned and dried tempered glass plate, spread lithium silicate fire retardant liquid, and let it air dry naturally for 48 hours to form a cured film with a water content of 35% and a thickness of 3mm. Then remove the water-blocking adhesive strips. The lithium silicate fire retardant liquid includes, by weight, 40 parts of lithium silicate (modulus 3.5), 5 parts of glycerin, 1 part of ammonium polyphosphate, 2 parts of urea, 0.3 parts of defoamer and 51.7 parts of water.

[0096] (2) Place the tempered glass plate with the cured film facing up in the laminating liquid, cover the top surface with a second tempered glass plate of the same size, and then laminate the sheets together using a press. The lamination pressure is 1 MPa, and the laminating liquid is isopropanol, which completely immerses the sheets together.

[0097] (3) After holding the pressure for 8 hours, release the pressure, take out the composite glass, let it stand at room temperature for 1 day, and then use a scraper to remove the gel-like cured film on the edge to obtain the composite fireproof glass with 2 glass and 1 adhesive.

[0098] Example 11

[0099] This embodiment provides a method for preparing composite fire-resistant glass using liquid-bed lamination compatible with tempered glass, the method comprising the following steps:

[0100] (1) Apply water-blocking adhesive strips to the edges of the cleaned and dried tempered glass plate, spread a mixture of potassium silicate and sodium silicate fire retardant liquid, and let it air dry naturally for 48 hours to form a cured film with a water content of 25% and a thickness of 2mm. Then remove the water-blocking adhesive strips. The mixture of potassium silicate and sodium silicate fire retardant liquid comprises, by weight, 20 parts of potassium silicate-sodium silicate mixture (modulus 5.5, potassium-sodium ratio 2), 5 parts of glycerin, 1 part of ammonium polyphosphate, 2 parts of urea, 0.3 parts of defoamer and 71.7 parts of water.

[0101] (2) The tempered glass plate is placed in the laminating liquid with the cured film facing up. After covering the top surface with a second tempered glass plate of the same size, the plates are laminated together using a press. The lamination pressure is 3 MPa, and the laminating liquid is ethanol, which completely immerses the plates.

[0102] (3) After holding the pressure for 8 hours, release the pressure, take out the composite glass, let it stand at room temperature for 4 days, and then use a scraper to remove the gel-like cured film on the edge to obtain the composite fireproof glass with 2 glass and 1 adhesive.

[0103] Example 12

[0104] This embodiment provides a method for preparing composite fire-resistant glass using liquid-bed lamination compatible with tempered glass, the method comprising the following steps:

[0105] (1) Apply water-blocking adhesive strips to the edges of the cleaned and dried tempered glass plate, spread potassium silicate fire retardant liquid, and let it air dry naturally for 48 hours to form a cured film with a water content of 15% and a thickness of 2mm. Then remove the water-blocking adhesive strips. The potassium silicate fire retardant liquid includes, by weight, 20 parts of potassium silicate (modulus 5), 5 parts of glycerin, 1 part of ammonium polyphosphate, 2 parts of borax, 0.3 parts of defoamer and 71.7 parts of water.

[0106] (2) Place the tempered glass plate with the cured film facing up in the laminating liquid, cover the top surface with a second tempered glass plate of the same size, and then laminate the sheets together using a press. The lamination pressure is 8 MPa, and the laminating liquid is isopropanol:ethanol (1:1) and completely immerses the sheets together.

[0107] (3) After holding the pressure for 20 hours, release the pressure, take out the composite glass and let it stand at room temperature for 5 days. Then use a scraper to remove the gel-like cured film on the edge to obtain the composite fireproof glass with 2 glass and 1 adhesive.

[0108] Example 13

[0109] This embodiment provides a method for preparing composite fire-resistant glass using liquid-bed lamination compatible with tempered glass, the method comprising the following steps:

[0110] (1) Apply water-blocking adhesive strips to the edges of the cleaned and dried tempered glass plate, spread potassium silicate fire retardant liquid, and let it air dry naturally for 48 hours to form a cured film with a water content of 24% and a thickness of 2mm. Then remove the water-blocking adhesive strips. The potassium silicate fire retardant liquid includes, by weight, 30 parts of potassium silicate (modulus 3.5), 5 parts of glycerin, 5 parts of ammonium polyphosphate, 1 part of borax, 0.3 parts of defoamer and 58.7 parts of water.

[0111] (2) Place the tempered glass plate with the cured film facing up in the laminating liquid, cover the top surface with a second tempered glass plate of the same size, and then laminate the sheets together using a press. The lamination pressure is 1 MPa, and the laminating liquid is diethylene glycol:isopropanol (1:4) and the sheets are completely immersed in it.

[0112] (3) After holding the pressure for 5 hours, release the pressure, take out the composite glass, let it stand at room temperature for 1 day, and then use a scraper to remove the gel-like cured film on the edge to obtain the composite fireproof glass with 2 glass and 1 adhesive.

[0113] Example 14

[0114] This embodiment provides a method for preparing composite fire-resistant glass using liquid-bed lamination compatible with tempered glass, the method comprising the following steps:

[0115] (1) After cleaning and drying, apply water-blocking strips to the edges of the two tempered glass plates respectively, spread potassium silicate fire retardant liquid on each plate, and let them air dry naturally for 48 hours to form a cured film with a water content of 35% and a thickness of 2mm. Then remove the water-blocking strips. The potassium silicate fire retardant liquid includes, by weight, 30 parts of potassium silicate (modulus 3.5), 5 parts of glycerin, 1 part of ammonium polyphosphate, 2 parts of borax, 0.3 parts of defoamer and 61.7 parts of water.

[0116] (2) Two tempered glass plates with curing films are stacked in the laminating liquid with the curing films facing upwards. A third tempered glass plate of the same size is then placed on top and laminated together using a press. The lamination pressure is 5 MPa and the laminating liquid is ethanol, which completely immerses the laminated plates.

[0117] (3) After holding the pressure for 15 hours, release the pressure, take out the composite glass, let it stand at room temperature for 6 days, and then use a scraper to remove the gel-like cured film on the edge to obtain the composite fireproof glass with 3 glass and 2 adhesive.

[0118] Example 15

[0119] This embodiment provides a method for preparing composite fire-resistant glass using liquid-bed lamination compatible with tempered glass, the method comprising the following steps:

[0120] (1) After cleaning and drying, water-blocking strips were attached to the edges of the five tempered glass plates, and potassium silicate fire retardant liquid was spread on each plate. After air drying for 48 hours to form a cured film with a water content of 35% and a thickness of 2mm, the water-blocking strips were removed. The potassium silicate fire retardant liquid included, by weight, 30 parts of potassium silicate (modulus 3.5), 5 parts of glycerin, 1 part of ammonium polyphosphate, 2 parts of borax, 0.3 parts of defoamer and 61.7 parts of water.

[0121] (2) Five tempered glass plates with curing film are stacked in the laminating liquid with the curing film facing up. A sixth tempered glass plate of the same size is then placed on top and laminated together using a press. The lamination pressure is 5 MPa and the laminating liquid is ethanol, which completely immerses the laminated plates.

[0122] (3) After holding the pressure for 20 hours, release the pressure, take out the composite glass and let it stand at room temperature for 6 days. Then, use a scraper to remove the gel-like cured film on the edge to obtain the composite fireproof glass with 6 glass and 5 adhesive.

[0123] Example 16

[0124] This embodiment provides a method for preparing composite fireproof glass using liquid lamination compatible with tempered glass. Except for the curing film thickness of 0.1 mm, the method is the same as in Embodiment 1.

[0125] Example 17

[0126] This embodiment provides a method for preparing composite fireproof glass using liquid lamination compatible with tempered glass. Except for the curing film thickness of 4 mm, the method is the same as that in Embodiment 1.

[0127] Example 18

[0128] This embodiment provides a method for preparing composite fireproof glass using liquid lamination compatible with tempered glass. The method is the same as in Embodiment 1, except that the water content of the cured film is 10%.

[0129] Example 19

[0130] This embodiment provides a method for preparing composite fireproof glass using liquid lamination compatible with tempered glass. The method is the same as in Example 1, except that the water content of the cured film is 40%.

[0131] Comparative Example 1

[0132] This comparative example provides a method for preparing composite fireproof glass by liquid lamination compatible with tempered glass. Except for lamination in the atmosphere, the method is the same as in Example 1.

[0133] Test methods

[0134] All test requirements met the national standard GB 15763.1-2009. The visible light transmittance of the composite fireproof glass provided in Examples 1-19 and Comparative Example 1 was tested according to the national standard GB / T 2680-2021. The hardness of the fireproof gel was tested using a Shore hardness tester. Its low-temperature resistance was tested using a temperature control device. Its radiation resistance was tested according to the national standard GB / T 5137.3 2020. The test results are shown in Table 1.

[0135] According to the national standard GB / T 12513-2006, the appearance quality and fire resistance limit of the fireproof glass in Examples 1-19 and Comparative Example 1 were tested, and the test results are shown in Table 2.

[0136] Test Results

[0137] Table 1

[0138] Examples and Comparative Examples Visible light transmittance (%) Hardness (HD) Low temperature resistance (24h) Visible light transmittance after irradiation (%) Example 1 88.5 93 -45℃ 86.0 Example 2 88.2 90 -50℃ 86.2 Example 3 88.0 92 -45℃ 86.1 Example 4 88.3 93 -45℃ 85.9 Example 5 88.6 95 -50℃ 86.3 Example 6 86.8 92 -45℃ 83.9 Example 7 88.1 94 -50℃ 85.8 Example 8 88.4 92 -40℃ 86.1 Example 9 88.3 91 -50℃ 86.0 Example 10 87.8 92 -40℃ 84.6 Example 11 88.1 92 -50℃ 85.8 Example 12 87.8 93 -50℃ 84.9 Example 13 87.9 93 -50℃ 84.3 Example 14 85.3 92 -45℃ 82.7 Example 15 83.9 93 -45℃ 80.9 Example 16 89.5 93 -45℃ 88.1 Example 17 86.1 89 -45℃ 83.3 Example 18 88.6 98 -50℃ 87.0 Example 19 88.2 81 -25℃ 81.3 Comparative Example 1 80.1 92 -45℃ 69.2

[0139] Table 2

[0140] Examples and Comparative Examples Appearance quality Insulation duration (min) Fire resistance integrity (min) Example 1 Clear and free of microbubbles 20 120 Example 2 Clear and free of microbubbles 19 120 Example 3 Clear and free of microbubbles 15 120 Example 4 Clear and free of microbubbles 23 120 Example 5 Clear and free of microbubbles 25 120 Example 6 Clear and free of microbubbles 28 120 Example 7 Clear and free of microbubbles 20 120 Example 8 Clear and free of microbubbles 23 120 Example 9 Clear and free of microbubbles 18 120 Example 10 Clear and free of microbubbles 27 120 Example 11 Clear and free of microbubbles 22 120 Example 12 Clear and free of microbubbles 21 120 Example 13 Clear and free of microbubbles 23 120 Example 14 Clear and free of microbubbles 40 180 Example 15 Clear and free of microbubbles 92 210 Example 16 Clear and free of microbubbles 5 120 Example 17 A small number of microbubbles at the edge 31 120 Example 18 A small number of microbubbles at the edge 18 120 Example 19 Clear and free of microbubbles 21 120 Comparative Example 1 Numerous microbubbles 12 120

[0141] The test results show that:

[0142] (1) As can be seen from Examples 1 to 15, the present invention can effectively meet the needs of preparing composite fireproof glass with different glass substrate types and different adhesive layers by using the pre-laying fireproof liquid and liquid lamination process; the pre-laying process can form a transparent curing film with uniform thickness and excellent light transmittance. The silicon-based fireproof liquid itself has good light transmittance. Combined with the low water content curing state, it significantly improves the low temperature resistance. The final composite fireproof glass can achieve a light transmittance of more than 83%, a low temperature resistance of more than -40℃, and stable weather resistance, which can be adapted to various indoor and outdoor application scenarios.

[0143] (2) As can be seen from Examples 1 and 16-19, the present invention further optimizes the thickness and moisture content of the cured film, avoiding local exposure of the substrate caused by excessively thin cured film or uneven shrinkage of the adhesive layer caused by excessively thick cured film. The balanced moisture content can improve weather resistance while ensuring the lamination microbubble discharge effect, and can better balance weather resistance and appearance quality.

[0144] (3) As can be seen from Example 1 and Comparative Example 1, the present invention can significantly reduce the generation of microbubbles by using the liquid lamination method. However, when the liquid lamination process is not used, the lamination process is prone to introducing bubbles, which leads to a decrease in appearance quality, light transmittance and weather resistance.

[0145] In summary, this invention achieves the technical effects of strong compatibility, defect-free appearance, high light transmittance, and stable fire resistance in the preparation of composite fireproof glass through a combination of fire-retardant liquid curing film and liquid-layer lamination, which can meet the application needs of fireproof glass in different scenarios.

[0146] The applicant declares that the above description is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention fall within the protection and disclosure scope of the present invention.

Claims

1. A method for preparing composite fireproof glass using liquid lamination compatible with tempered glass, characterized in that, The method includes the following steps: (1) Fire retardant liquid is spread on at least one first glass substrate, and solvent is removed to form a cured film; (2) The first glass substrate is stacked in the laminating liquid with the cured film facing upward, and the second glass substrate is covered on the top surface and then laminated underwater to obtain a laminate, wherein the laminating liquid completely immerses the laminate; (3) After taking out the composite glass and letting it stand for aging, post-processing is carried out to obtain the composite fireproof glass.

2. The method according to claim 1, characterized in that, The first glass substrate consists of 1 to 9 pieces.

3. The method according to claim 1 or 2, characterized in that, The fire retardant liquid includes silicate fire retardant liquid; Preferably, the silicate fire retardant liquid comprises, by weight, 20-35 parts silicate, 2-15 parts charring agent, 1-5 parts flame retardant, 1-5 parts fire retardant additive, 0.3-1 part defoamer, and 50-80 parts water.

4. The method according to any one of claims 1 to 3, characterized in that, The silicate is M2O·(SiO2). n M is a metallic element, which includes any one or a combination of at least two of sodium, potassium and lithium, and the modulus n of the silicate is 3-6. Preferably, the char-forming agent includes any one or a combination of at least two of ethylene glycol, glycerol, sorbitol, pentaerythritol, sucrose, and fructose; Preferably, the flame retardant comprises any one or a combination of at least two of ammonium polyphosphate, sodium polyphosphate, melamine phosphate, and water-soluble phosphate ester; Preferably, the refractory additive includes any one or a combination of at least two of borax, urea and melamine; Preferably, the defoamer comprises polyether-modified silicone.

5. The method according to any one of claims 1 to 4, characterized in that, The cured film has a water content of 15-35 wt%. Preferably, the thickness of the cured film is 0.5-3 mm.

6. The method according to any one of claims 1 to 5, characterized in that, The first glass substrate has water-resistant adhesive strips attached to its four edges to maintain the thickness of the fire retardant liquid. The waterproof adhesive strips are removed after the solvent is removed.

7. The method according to any one of claims 1 to 6, characterized in that, The laminating fluid includes any one or a combination of at least two of the following: pure water, ethanol, isopropanol, ethylene glycol, diethylene glycol, glycerol, and propylene glycol.

8. The method according to any one of claims 1 to 7, characterized in that, The pressure of the subsurface lamination is 1-10 MPa.

9. The method according to any one of claims 1 to 8, characterized in that, The first glass substrate and the second glass substrate are pretreated glass; Preferably, the pretreatment includes cleaning to remove surface dirt and drying; Preferably, the glass comprises tempered glass or float glass.

10. The method according to any one of claims 1 to 9, characterized in that, The aging and settling time is 1-15 days; Preferably, the static aging process is carried out at room temperature; Preferably, the post-processing includes removing the gel-like cured film that has been squeezed out from the edges.

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