CN112194986B - Composite glass flame-retardant heat-insulation liquid and production process and application thereof - Google Patents

Composite glass flame-retardant heat-insulation liquid and production process and application thereof Download PDF

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CN112194986B
CN112194986B CN202011141393.XA CN202011141393A CN112194986B CN 112194986 B CN112194986 B CN 112194986B CN 202011141393 A CN202011141393 A CN 202011141393A CN 112194986 B CN112194986 B CN 112194986B
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composite glass
water glass
flame
glass
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CN112194986A (en
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崔金海
施文福
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Henan Chengxin Sealing New Material Technology Research Institute Co ltd
Shangqiu Normal University
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Henan Chengxin Sealing New Material Technology Research Institute Co ltd
Shangqiu Normal University
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J1/00—Adhesives based on inorganic constituents
    • C09J1/02—Adhesives based on inorganic constituents containing water-soluble alkali silicates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J1/00—Adhesives based on inorganic constituents
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08—Macromolecular additives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/306—Resistant to heat
    • B32B2307/3065—Flame resistant or retardant, fire resistant or retardant

Abstract

The invention relates to a composite glass flame-retardant heat-insulating liquid and a production process and application thereof. The composite glass flame-retardant heat-insulating liquid comprises: compounding 45 to 50 parts of water glass solution, 48 to 53 parts of compound nano silicon dioxide emulsion, 1 to 3 parts of defoaming agent and 1 to 5 parts of inorganic salt auxiliary curing agent; the compound water glass solution comprises: 6-12 parts of potassium hydroxide, 1-5 parts of a toughening agent, and 83-93 parts of a sodium water glass solution or a potassium water glass solution; the compound nano silicon dioxide emulsion comprises: 1 to 5 parts of polymer monomer A, 3 to 8 parts of polyester additive, 82 to 95 parts of nano silica sol and 1 to 5 parts of polymer monomer B. The curing time of the flame-retardant heat-insulating liquid prepared by the invention is controllable, and the transparent enamel layer obtained by curing has high bonding strength, good high-low temperature performance and no micro-bubbles; simple production process, low cost and good fireproof performance. The performance of the composite glass completely meets the requirements of national standards, and the composite glass has good performance in the aspects of product appearance, cold resistance, ultraviolet irradiation resistance and the like.

Description

Composite glass flame-retardant heat-insulation liquid and production process and application thereof
Technical Field
The invention relates to a composite glass flame-retardant heat-insulating liquid, a production process and application, and belongs to the field of safety glass production.
Background
The safety glass is a building outer wall or door and window glass with flame-retardant, heat-insulation and heat-insulation functions, and can be kept for a long time without cracking under the high-temperature condition of a fire, so that the spread of flame and smoke is effectively prevented, the fire condition can be found in the first time, the people suffering from the fire can be guaranteed to have enough time to evacuate from the site, and the time is won for the disaster relief work. The composite fireproof glass is a development direction of safety glass, and is a glass combination formed by bonding two or more pieces of common plate glass by using a transparent flame-retardant heat-insulating adhesive or spraying composite fireproof glass liquid, when a fire disaster occurs, the composite glass on the fire head side is exploded when encountering high temperature, and the exposed flame-retardant heat-insulating adhesive interlayer absorbs high heat released by flame combustion, foams and expands to form a white opaque flame-retardant heat-insulating adhesive plate, so that the integrity of glass on the fire back side is ensured, flame, smoke and toxic gas are effectively isolated, and good isolation, bonding and mechanical properties are presented. In the composite safety glass, the quality of the flame-retardant heat-insulating adhesive is the key for determining the comprehensive performance of the composite safety glass.
The flame-retardant heat-insulating glue for the composite safety glass at the present stage has various defects on the flame-retardant heat-insulating property, such as a large number of micro bubbles are easily generated in the curing process, the apparent quality of the composite fireproof glass is directly influenced, and the flame-retardant heat-insulating property, the optical property, the hardness and the toughness of the composite glass are seriously influenced; in addition, the preparation process is complex, the preparation period is long, the storage time is short, the storage condition is harsh, and the problems that the flame-retardant heat-insulating adhesive product cannot be filled into the composite glass interlayer, the flame-retardant heat-insulating liquid product is denatured and the like often occur; the surface of the prepared flame-retardant heat-insulation film is difficult to achieve the smoothness, gaps which are difficult to overcome exist among the composite glass sheets, the use effect and the service life of the composite fireproof glass are seriously influenced, and the commercial application requirements are difficult to achieve. Therefore, there is a need for further development of a composite glass flame-retardant and heat-insulating liquid and composite glass with simple production process, no microbubbles and good fire resistance.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the composite glass flame-retardant heat-insulating liquid and the production process and the application thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
the composite glass flame-retardant heat-insulating liquid comprises the following raw materials in parts by weight: compounding 45-50 parts of water glass solution, 48-53 parts of compounded nano silicon dioxide emulsion, 1-3 parts of defoaming agent and 1-5 parts of inorganic salt auxiliary curing agent;
the composite water glass solution comprises, by weight, 6 to 12 parts of potassium hydroxide, 1 to 5 parts of a toughening agent, and 83 to 93 parts of a sodium water glass solution or a potassium water glass solution;
the compound nano-silica emulsion comprises, by weight, 1-5 parts of a polymer monomer A, 3-8 parts of a polyester auxiliary agent, 82-95 parts of a nano-silica sol and 1-5 parts of a polymer monomer B.
SiO in the sodium silicate 2 With Na 2 The molar ratio of O is 3:1; siO in potassium water glass 2 And K 2 The molar ratio of O is 3:1.
the polymer monomer A is any one of or a mixture of two or more of vinyl pyrrolidone, vinyl acetate, acrylic acid, methacrylic acid, N-methacrylamide, ethyl acrylate, propyl acrylate and butyl acrylate; the polymer monomer B is methyl methacrylate, ethyl methacrylate or butyl methacrylate.
The defoaming agent is organic silicon emulsion or modified organic silicon emulsion.
The preparation method of the modified organic silicon emulsion comprises the following steps: according to parts by weight, 30 parts of water-based organic silicon 3-glycidyl ether oxygen propyl trimethoxy silane KH-560 and 10 parts of KI are added into 100 parts of BYK-024 organic silicon defoaming agent, and stirring reaction is carried out for 6 hours at the temperature of 70 ℃ to obtain the organic silicon defoaming agent.
The polyester auxiliary agent is any one of ethylene glycol, glycerol and pentaerythritol, or a mixture of the two or more of the ethylene glycol, the glycerol and the pentaerythritol; the toughening agent is any one of sorbitol, mannitol, lactitol, glucose, sucrose and xylitol, or a mixture of the two or more; the inorganic salt auxiliary curing agent is NaCl, KCl, naI, KI and NaNO 3 、KNO 3 、Na 3 PO 4 、K 3 PO 4、 NaH 2 PO 4 、Na 2 HPO 4 、KH 2 PO 4 、K 2 HPO 4 Either one of, orA mixture of two or more thereof.
The production process of the composite glass flame-retardant heat-insulating liquid comprises the following steps:
(1) Weighing the raw materials according to the proportion, uniformly mixing potassium hydroxide, a flexibilizer and sodium or potassium water glass, and centrifugally separating at 25 ℃ to remove insoluble impurities to obtain a compound water glass solution for later use;
(2) Uniformly mixing the polymer monomer A, the polyester additive and the nano-silica sol, fully stirring for 0.5-2 hours at 25-40 ℃, adding the polymer monomer B, and fully stirring for 0.5-1 hour to obtain a compound nano-silica emulsion for later use;
(3) And (2) uniformly mixing the compound water glass solution, the compound nano silicon dioxide emulsion, the defoaming agent and the inorganic salt auxiliary curing agent, wherein the solution is changed into milky from transparent, stirring for 0.5-1 h at 25-40 ℃, changing to 200Pa of vacuum degree after the viscosity of the mixed solution is reduced and the mixed solution is changed into transparent again, stirring for 20 min at the speed of 100-150 rpm, standing for defoaming in a vacuum state, and filtering on a 100-mesh screen to obtain the composite glass flame-retardant heat-insulating liquid.
The production process of the composite glass flame-retardant heat-insulating liquid comprises the following steps:
(1) Weighing the raw materials according to the proportion, uniformly mixing potassium hydroxide, a flexibilizer and sodium or potassium water glass, and centrifugally separating at 25 ℃ to remove insoluble impurities to obtain a compound water glass solution for later use;
(2) Uniformly mixing a polymer monomer A, a polyester additive and nano-silica sol, fully stirring for 0.5-2 hours at 25-40 ℃, adding a polymer monomer B, and fully stirring for 0.5-1 hour to obtain a compound nano-silica emulsion for later use;
(3) And uniformly mixing the compound water glass solution, the compound nano silicon dioxide emulsion and the defoaming agent, changing the solution from transparent to milky at the moment, stirring at 25-40 ℃, adding the inorganic salt auxiliary curing agent after the viscosity of the mixed solution is reduced and the mixed solution is changed into transparent again, continuously stirring for 0.5-1 h, changing to the vacuum degree of 200Pa, stirring for 20 min at the speed of 100-150 rpm, standing for defoaming in a vacuum state, and filtering on a 100-mesh screen to obtain the composite glass flame-retardant heat-insulating liquid.
The composite glass flame-retardant heat-insulating liquid is applied to the preparation of composite glass.
The preparation method of the composite glass comprises the following steps: and pouring the composite glass flame-retardant heat-insulating liquid into a toughened composite glass cavity, wherein the thickness of the cavity is 2-5 mm, the periphery of the composite glass is sealed by adopting an impervious and leakproof single-channel sealant, and curing for 3-7 hours to obtain the composite glass.
The invention has the beneficial effects that:
according to the composite glass flame-retardant heat-insulating liquid, the modified organic silicon defoaming agent and the auxiliary inorganic salt curing agent are added, so that the gelation time of the heat-insulating liquid filled composite glass can be flexibly regulated, the curing time is controllable, the transparent enamel layer obtained by curing is high in bonding strength, and the obtained composite glass is good in high-temperature and low-temperature performance, free of micro bubbles, simple in production process, low in cost and good in fireproof performance. The method comprises the following specific steps:
(1) According to the invention, the modified organic silicon defoaming agent is added into the raw materials, so that bubbles in the high-viscosity mixed solution can be effectively removed, the transparent gel without the microbubbles can be obtained, the gelation time of the heat insulation liquid can be controlled, the gelation temperature can be reduced, and the industrial production of the heat insulation liquid and the filling requirement of the heat insulation liquid of the composite glass are facilitated.
(2) According to the invention, the alkenyl carboxylic acid (ester) or alkenyl amide polymer monomer is added into the raw materials, and the polymerization activity of the alkenyl carboxylic acid (ester) or alkenyl amide polymer monomer under an alkaline condition is utilized, so that the flame-retardant heat-insulating liquid can be ensured to have a certain degree of in-situ polymerization reaction in the formed inorganic gel without adding any polymerization reaction initiator, the viscosity of the inorganic gel is reduced, and the impact strength of the inorganic gel is improved. Because the existence of excessive organic polymer can reduce the bonding performance of inorganic gel in the composite glass to the glass, the dosage of all polymer monomers in the formula of the flame-retardant heat-insulating liquid is controlled to be not more than 5 percent.
(3) According to the invention, inorganic salt auxiliary curing agent is added into the raw materials, and the weakening effect of the electrolyte counter ions on the double electric layers of the micelle is ensured according to the theory of double electric layers of the micelle, so that the size of colloidal particles can be effectively reduced, the thermal motion among colloidal particles is intensified, the coagulation effect among colloidal particles is promoted, and after the composite glass is filled, the thermal insulation liquid is favorable for forming transparent gel with adjustable curing time. Because the light transmittance of formed gel is obviously reduced due to excessive use of the inorganic salt, the use amount of the inorganic salt auxiliary curing agent controlled by the flame-retardant heat-insulating liquid is generally not more than 5%.
(4) The raw materials of the invention are added with the polyhydric alcohol with strong activity such as glycol, glycerol, pentaerythritol and the like as the polyester additive, which is beneficial to the formation of the polyhydric alcohol silicate polymer in the gelation process of the fireproof heat-insulating liquid. The generation of the polyester compound not only has effective crosslinking and curing effects on inorganic glass gel and enhances the strength of the gel, but also enhances the low-temperature resistance of the sol, and the glass atomization phenomenon is not easy to occur even at the temperature of minus 20 ℃. By adding higher molecular weight polyols such as sorbitol, mannitol, lactitol, glucose, sucrose, xylitol and the like as the toughening agent, the toughness of the fireproof heat-insulating liquid in the curing process can be enhanced, and the deformation resistance of the composite glass product in the outdoor environment is improved.
(5) The performance of the composite glass filled with the flame-retardant heat-insulating liquid completely meets the national standard requirements, and the composite glass has good performances in the aspects of product appearance, cold resistance, ultraviolet irradiation resistance and the like.
Drawings
FIG. 1 composite glass filled with flame-retardant and heat-insulating liquid according to example 1 of the present invention;
FIG. 2 shows the glass foam state of the flame-retardant heat-insulating liquid of example 1 of the present invention after dehydration by heating at 200 ℃.
Detailed Description
The following examples further illustrate embodiments of the present invention in detail.
The composite glass flame-retardant heat-insulating liquid of the invention has the following raw material requirements:
potassium hydroxide: the purity is 90 wt%; the content of the nano-silica sol is 30 wt% or 40 wt%;
sodium water glass: siO 2 2 With Na 2 Mole of OThe molar ratio is 3:1, content 38 wt%, technical grade;
potassium water glass: siO 2 2 And K 2 The molar ratio of O is 3:1, content 38 wt%, technical grade;
the purities of the polyester auxiliary agent, the toughening agent, the inorganic salt auxiliary curing agent and the polymer monomer are analytically pure;
the preparation method of the modified organic silicon emulsion comprises the following steps: according to parts by weight, 30 parts of water-based organic silicon 3-glycidyl ether oxygen propyl trimethoxy silane KH-560 and 10 parts of KI inorganic salt are added into 100 parts of BYK-024 organic silicon defoaming agent, and stirred and reacted for 6 hours at 70 ℃ to obtain the organic silicon defoaming agent.
Example 1
The composite glass flame-retardant heat-insulating liquid comprises the following raw materials: 45 kg of compound water glass solution, 53 kg of compound nano silicon dioxide emulsion, 1 kg of defoaming agent modified organic silicon emulsion and 1 kg of KCl;
wherein, every 100 kg of the compound water glass solution comprises: 10 kg of potassium hydroxide tablets, 2.5 kg of toughener sorbitol and 87.5 kg of sodium water glass solution;
every 100 kg of the compound nano silicon dioxide emulsion comprises: 1 kg of vinyl acetate, 5 kg of polyester auxiliary agent glycerol, 93 kg of acidic nano silica sol (with the purity of 40 wt%) and 1 kg of butyl methacrylate.
The production process of the composite glass flame-retardant heat-insulating liquid comprises the following steps:
(1) Weighing the raw materials according to a ratio, uniformly mixing potassium hydroxide, sorbitol and sodium silicate, and centrifugally separating at 25 ℃ to remove insoluble impurities to obtain a compound water glass solution for later use;
(2) Uniformly mixing vinyl acetate, glycerol and acidic nano-silica sol, fully stirring for 0.5h at 40 ℃, adding butyl methacrylate, and fully stirring for 0.5h to obtain a compound nano-silica emulsion for later use;
(3) And (2) uniformly mixing the compound water glass solution, the compound nano silicon dioxide emulsion, the defoaming agent modified organosilicon emulsion and KCl, wherein the solution is changed into milk white from transparent, stirring for 0.5h at 40 ℃, changing to a vacuum degree of 200Pa after the viscosity of the mixed solution is reduced and is changed into transparent again, stirring for 20 min at a speed of 150 rpm, cooling to 25 ℃ in a vacuum state, slowly raising to normal pressure, standing for defoaming, and filtering on a 100-mesh screen to obtain the composite glass flame-retardant heat-insulating liquid.
And pouring the prepared composite glass flame-retardant heat-insulating liquid into a toughened composite glass cavity, wherein the thickness of the cavity is 2 mm, the periphery of the composite glass is sealed by anti-seepage and anti-leakage CX103 hollow glass single-channel sealant, curing in a drying oven at 60 ℃, and taking out after 3 hours to obtain the microbubble-free and transparent composite glass.
As shown in figure 1, the composite glass filled with the flame-retardant heat-insulating liquid has no tiny bubbles and transparency of more than 97 percent, and has no phenomena of color change, liquid leakage, fogging and the like after being placed in an outdoor environment for 2 years. As shown in figure 2, after the flame-retardant heat-insulating liquid is heated at 200 ℃ and loses water, rich and compact vitreous enamel is generated on the glass surface facing fire, and the flame-retardant heat-insulating liquid can effectively isolate the fire scene, shield heat radiation and prevent toxic smoke from diffusing.
The composite glass of the embodiment is subjected to performance detection, and the main indexes are shown in the following table 1.
TABLE 1 product Performance index of example 1
Figure DEST_PATH_IMAGE002
Wherein, the light transmittance is the finished product light transmittance of the composite glass finished product at 25 ℃; the bonding strength is 200 ℃, the composite glass is baked for 1 hour, and after the composite glass is prevented from being gelled and foamed, the bonding strength between the fireproof glue and the glass is realized; the aging performance is that an ozone-free quartz tube type medium-pressure mercury vapor arc lamp with the power of 750W is used, the sample is irradiated for 100 hours at the temperature of 45 ℃ and at the distance of 230mm from the lamp axis, and the obtained light transmittance change value is obtained; the low-temperature performance is the light transmittance value when the composite glass is placed in a refrigerator and cooled to-20 ℃. The performance metrics of tables 2-5 below are similar.
Example 2
The composite glass flame-retardant heat-insulating liquid comprises the following raw materials: 48 kg of compound water glass solution, 49.5 kg of compound nano silicon dioxide emulsion, 1.5 kg of defoaming agent modified organic silicon emulsion and 2 kg of KI;
wherein every 100 kg of the compound water glass solution comprises: 8 kg of potassium hydroxide tablets, 2 kg of toughening agent lactitol and 90 kg of potassium water glass solution;
every 100 kg of the compound nano silicon dioxide emulsion comprises: 2 kg of acrylic acid, 8 kg of polyester additive glycerol, 89 kg of acidic nano silica sol (with the purity of 40 wt%) and 1 kg of butyl methacrylate.
The production process of the composite glass flame-retardant heat-insulating liquid comprises the following steps:
(1) Weighing the raw materials according to the proportion, uniformly mixing potassium hydroxide, lactitol and potassium water glass, and centrifugally separating at 25 ℃ to remove insoluble impurities to obtain a compound water glass solution for later use;
(2) Uniformly mixing acrylic acid, glycerol and acidic nano-silica sol, fully stirring for 1 h at 25 ℃, adding butyl methacrylate, and fully stirring for 0.5h to obtain a compound nano-silica emulsion for later use;
(3) And (3) uniformly mixing the compound water glass solution, the compound nano silicon dioxide emulsion, the defoaming agent modified organic silicon emulsion and KI, wherein the solution is changed into milky white from transparent, stirring for 1 h at 25 ℃, changing to the vacuum degree of 200Pa after the viscosity of the mixed sol is reduced and is changed into transparent again, stirring for 20 min at the speed of 100 rpm, standing for defoaming in a vacuum state, and filtering by using a 100-mesh screen to obtain the composite glass flame-retardant heat-insulating liquid.
And pouring the prepared composite glass flame-retardant heat-insulating liquid into a toughened composite glass cavity, wherein the thickness of the cavity is 3 mm, the periphery of the composite glass is sealed by adopting impervious and leakproof single-channel sealant, curing at normal temperature, and taking out after 7 hours to obtain the normally cured transparent composite glass without microbubbles.
The obtained composite glass is detected, and the main performance indexes are as the following table 2:
TABLE 2 Properties of the products of example 2
Figure DEST_PATH_IMAGE004
Example 3
The composite glass flame-retardant heat-insulating liquid comprises the following raw materials: 50 kg of compound water glass solution, 48 kg of compound nano silicon dioxide emulsion, 2 kg of defoaming agent modified organic silicon emulsion and KH 2 PO 4 1 kg；
Wherein every 100 kg of the compound water glass solution comprises: 10 kg of potassium hydroxide tablets, 2 kg of toughening agent xylitol and 88 kg of potassium water glass solution;
every 100 kg of the compound nano silicon dioxide emulsion comprises: 1 kg of acrylic acid, 1 kg of N-methacrylamide, 6 kg of polyester auxiliary agent pentaerythritol, 90 kg of acidic nano silica sol (the content is 40wt percent), and 2 kg of ethyl methacrylate.
The production process of the composite glass flame-retardant heat-insulating liquid comprises the following steps:
(1) Weighing the raw materials according to the proportion, uniformly mixing potassium hydroxide, xylitol and potassium water glass, and centrifugally separating at 25 ℃ to remove insoluble impurities to obtain a compound water glass solution for later use;
(2) Uniformly mixing acrylic acid, N-methacrylamide, pentaerythritol and acidic nano-silica sol, fully stirring for 1 h at 35 ℃, adding ethyl methacrylate, and fully stirring for 1 h to obtain a compound nano-silica emulsion for later use;
(3) Mixing the above compound water glass solution, compound nano silicon dioxide emulsion and defoaming agent modified organosilicon emulsion uniformly, at this moment, the solution turns to milk white from transparent, stirring at 25 deg.C, when the viscosity of the mixed sol is reduced and turned to transparent again, adding KH 2 PO 4 And continuously stirring for 1 h, changing to the vacuum degree of 200Pa, stirring at the speed of 100 rpm for 20 min, standing and defoaming in the vacuum state, and filtering with a 100-mesh screen to obtain the composite glass flame-retardant heat-insulating liquid.
And pouring the prepared composite glass flame-retardant heat-insulating liquid into a toughened composite glass cavity, wherein the thickness of the cavity is 3 mm, the periphery of the composite glass is sealed by adopting impervious and leakproof single-channel sealant, curing at normal temperature, and taking out after 4 hours to obtain the microbubble-free transparent composite glass.
The inorganic salt is used as an auxiliary curing agent, and can prolong the time for converting the heat insulation liquid from opaque to transparent solution, so that the inorganic salt can be flexibly added before or after the heat insulation liquid is converted into transparent solution according to different requirements of working time and storage time.
The obtained composite glass is detected, and the main performance indexes are as follows in the following table 3:
TABLE 3 Properties of the products of example 3
Figure DEST_PATH_IMAGE006
Example 4
The composite glass flame-retardant heat-insulating liquid comprises the following raw materials: 46 kg of compound water glass solution, 50 kg of compound nano silicon dioxide emulsion, 1.5 kg of defoaming agent modified organic silicon emulsion and K 3 PO 4 2.5 kg；
Wherein each 100 kg of the compound water glass solution comprises: 7 kg of potassium hydroxide tablets, 3 kg of toughener sorbitol and 90 kg of sodium water glass solution;
every 100 kg of the compound nano silicon dioxide emulsion comprises: 1 kg of acrylic acid, 1 kg of N-methacrylamide, 1 kg of vinyl acetate, 5 kg of polyester auxiliary agent ethylene glycol, 90 kg of neutral nano silica sol (with the purity of 40 wt%) and 2 kg of butyl methacrylate.
The production process of the composite glass flame-retardant heat-insulating liquid comprises the following steps:
(1) Weighing the raw materials according to a ratio, uniformly mixing potassium hydroxide, sorbitol and sodium silicate, and centrifugally separating at 25 ℃ to remove insoluble impurities to obtain a compound water glass solution for later use;
(2) Uniformly mixing acrylic acid, N-methacrylamide, vinyl acetate, ethylene glycol and neutral nano-silica sol, fully stirring for 1 hour at the temperature of 30 ℃, adding butyl methacrylate, and fully stirring for 1 hour to obtain a compound nano-silica emulsion for later use;
(3) Mixing the above compound water glass solution, compound nano silicon dioxide emulsion and defoaming agent modified organosilicon emulsion uniformly, at this moment, the solution turns to milk white from transparent, stirring at 25 deg.C, when the viscosity of mixed sol is reduced and turned to transparent again, adding K 3 PO 4 And continuously stirring for 1 h, changing to the vacuum degree of 200Pa, stirring at the speed of 100 rpm for 20 min, standing for defoaming in the vacuum state, and filtering by using a 100-mesh screen to obtain the composite glass flame-retardant heat-insulating liquid.
And pouring the prepared composite glass flame-retardant heat-insulating liquid into a toughened composite glass cavity, wherein the thickness of the cavity is 5mm, the periphery of the composite glass is sealed by adopting an impervious and leakproof single-channel sealant, curing at room temperature, and taking out after 3 hours to obtain the transparent composite glass without microbubbles and with high toughness.
The obtained composite glass is detected, and the main performance indexes are as follows in the following table 4:
TABLE 4 Properties of the products of example 4
Figure DEST_PATH_IMAGE008
Example 5
The composite glass flame-retardant heat-insulating liquid comprises the following raw materials: 45 kg of compound water glass solution, 51 kg of compound nano silicon dioxide emulsion, 3 kg of defoaming agent modified organic silicon emulsion and 1 kg of NaCl;
wherein each 100 kg of the compound water glass solution comprises: 9 kg of potassium hydroxide tablets, 5 kg of toughening agent sucrose and 86 kg of potassium water glass solution;
every 100 kg of the compound nano silicon dioxide emulsion comprises: 2 kg of methacrylic acid, 2 kg of vinyl acetate, 5 kg of polyester auxiliary agent glycerol, 89 kg of alkaline nano silica sol (the content is 30wt percent), and 2 kg of ethyl methacrylate.
The production process of the composite glass flame-retardant heat-insulating liquid comprises the following steps:
(1) Weighing the raw materials according to the proportion, uniformly mixing potassium hydroxide, sucrose and potassium water glass, and centrifugally separating at 25 ℃ to remove insoluble impurities to obtain a compound water glass solution for later use;
(2) Uniformly mixing methacrylic acid, vinyl acetate, glycerol and alkaline nano-silica sol, fully stirring for 1 h at 30 ℃, adding ethyl methacrylate, and fully stirring for 1 h to obtain a compound nano-silica emulsion for later use;
(3) And (2) uniformly mixing the compound water glass solution, the compound nano silicon dioxide emulsion and the defoaming agent modified organic silicon emulsion, changing the solution from transparent to milky at the moment, stirring at 25 ℃, adding NaCl after the viscosity of the mixed sol is reduced and is changed into transparent again, continuously stirring for 1 h, changing to a vacuum degree of 200Pa, stirring at the speed of 150 rpm for 20 min, standing for defoaming in a vacuum state, and filtering on a 100-mesh screen to obtain the composite glass flame-retardant heat-insulating liquid.
And pouring the prepared composite glass flame-retardant heat-insulating liquid into a toughened composite glass cavity, wherein the thickness of the cavity is 2 mm, the periphery of the composite glass is sealed by adopting an impervious and leakproof single-channel sealant, curing at room temperature, taking out after 5 hours, and obtaining the brownish red transparent composite glass which is free of microbubbles, quick to cure, high in toughness and used for installing door and window glass of a private space due to the fact that colored polyester is formed by cane sugar and silica sol.
The obtained composite glass is detected, and the main performance indexes are as follows in the following table 5:
TABLE 5 Properties of example 5
Figure DEST_PATH_IMAGE010
As can be seen from table 5, the light transmittance of the composite glass product is less than 30%, which may be due to the fact that the composite glass appears brownish red due to the color change reaction between the heat insulating liquid and sucrose after the sucrose is added.
Example 6 analysis of Properties of composite glasses according to the invention
The relevant properties of the composite glasses of examples 1-5 were compared with the national standard GB15763.1-2009, table 6 below, according to the test methods and conditions of the national standard GB15763.1-2009, the revision GB50016-2014, GB/T5137.3.2002, GB/T12513.2006:
TABLE 6 Properties relating to the composite glasses of the invention
Figure DEST_PATH_IMAGE012
The performance of the composite glass completely meets the requirements of national standards, and the composite glass has good performance in the aspects of product appearance, cold resistance, ultraviolet irradiation resistance and the like.
In addition to the above examples, the present invention may also be modified such that polymer monomer A is any one of vinyl pyrrolidone, vinyl acetate, acrylic acid, methacrylic acid, N-methyl acrylamide, ethyl acrylate, propyl acrylate, butyl acrylate, or a mixture of two or more thereof; the polymer monomer B is methyl methacrylate, ethyl methacrylate or butyl methacrylate; the nano silica sol can be alkaline, acidic or neutral; the defoaming agent is organic silicon emulsion or modified organic silicon emulsion; the polyester auxiliary agent is any one of ethylene glycol, glycerol and pentaerythritol, or a mixture of the two or more of the two; the toughening agent is any one of sorbitol, mannitol, lactitol, glucose, sucrose and xylitol, or a mixture of the two or more of the sorbitol, the mannitol, the lactitol and the glucose; the inorganic salt auxiliary curing agent is NaCl, KCl, naI, KI and NaNO 3 、KNO 3 、Na 3 PO 4 、K 3 PO 4、 NaH 2 PO 4 、Na 2 HPO 4 、KH 2 PO 4 、K 2 HPO 4 Any one of them, or a mixture of two or more of them, and variations or combinations of such schemes can implement the present invention, which are not listed.

Claims (6)

1. The composite glass flame-retardant heat-insulating liquid is characterized by comprising the following raw materials in parts by weight: compounding 45 to 50 parts of water glass solution, 48 to 53 parts of compound nano silicon dioxide emulsion, 1 to 3 parts of defoaming agent and 1 to 5 parts of inorganic salt auxiliary curing agent;
the compounded water glass solution comprises, by weight, 6 to 12 parts of potassium hydroxide, 1 to 5 parts of a toughening agent, and 83 to 93 parts of a sodium water glass solution or a potassium water glass solution;
the compound nano silicon dioxide emulsion comprises, by weight, 1-5 parts of a polymer monomer A, 3-8 parts of a polyester auxiliary agent, 82-95 parts of a nano silicon dioxide sol and 1-5 parts of a polymer monomer B;
the defoaming agent is modified organic silicon emulsion, and the preparation method comprises the following steps: adding 30 parts by weight of water-based organic silicon 3-glycidyl ether oxygen propyl trimethoxy silane KH-560 and 10 parts by weight of KI into 100 parts by weight of BYK-024 organic silicon defoaming agent, and stirring and reacting for 6 hours at the temperature of 70 ℃ to obtain the water-based organic silicon defoaming agent;
the polymer monomer A is any one of or a mixture of two or more of vinyl pyrrolidone, vinyl acetate, acrylic acid, methacrylic acid, N-methacrylamide, ethyl acrylate, propyl acrylate and butyl acrylate; the polymer monomer B is methyl methacrylate, ethyl methacrylate or butyl methacrylate;
the polyester auxiliary agent is any one of ethylene glycol, glycerol and pentaerythritol, or a mixture of the two or more; the toughening agent is any one of sorbitol, mannitol, lactitol, glucose, sucrose and xylitol, or a mixture of the two or more of the sorbitol, the mannitol, the lactitol and the glucose; the inorganic salt auxiliary curing agent is NaCl, KCl, naI, KI and NaNO 3 、KNO 3 、Na 3 PO 4 、K 3 PO 4、 NaH 2 PO 4 、Na 2 HPO 4 、KH 2 PO 4 、K 2 HPO 4 Any one of them, or a mixture of two or more of them.
2. The composite glass flame-retardant heat-insulating liquid according to claim 1, wherein SiO in the sodium silicate 2 With Na 2 The molar ratio of O is 3:1; siO in potassium water glass 2 And K 2 The molar ratio of O is 3:1.
3. a process for producing a fire-retardant and heat-insulating composite glass liquid according to any one of claims 1 to 2, comprising the steps of:
(1) Weighing the raw materials according to the proportion, uniformly mixing potassium hydroxide, a flexibilizer and sodium water glass or potassium water glass, and then centrifugally separating at 25 ℃ to remove insoluble impurities to obtain a compound water glass solution for later use;
(2) Uniformly mixing a polymer monomer A, a polyester additive and nano-silica sol, fully stirring for 0.5-2 hours at 25-40 ℃, adding a polymer monomer B, and fully stirring for 0.5-1 hour to obtain a compound nano-silica emulsion for later use;
(3) And uniformly mixing the compound water glass solution, the compound nano silicon dioxide emulsion, the defoaming agent and the inorganic salt auxiliary curing agent, changing the solution from transparent to milky white, stirring for 0.5-1 h at 25-40 ℃, changing the mixed solution to a vacuum degree of 200Pa after the viscosity of the mixed solution is reduced and the mixed solution becomes transparent again, stirring for 20 min at a speed of 100-150 rpm, standing for defoaming in a vacuum state, and filtering on a 100-mesh screen to obtain the composite glass flame-retardant heat-insulating liquid.
4. A process for producing a fire-retardant and heat-insulating composite glass liquid according to any one of claims 1 to 2, comprising the steps of:
(1) Weighing the raw materials according to the proportion, uniformly mixing potassium hydroxide, a flexibilizer and sodium or potassium water glass, and centrifugally separating at 25 ℃ to remove insoluble impurities to obtain a compound water glass solution for later use;
(2) Uniformly mixing a polymer monomer A, a polyester additive and nano-silica sol, fully stirring for 0.5-2 hours at 25-40 ℃, adding a polymer monomer B, and fully stirring for 0.5-1 hour to obtain a compound nano-silica emulsion for later use;
(3) And uniformly mixing the compound water glass solution, the compound nano silicon dioxide emulsion and the defoaming agent, changing the solution from transparent to milky at the moment, stirring at 25-40 ℃, adding the inorganic salt auxiliary curing agent after the viscosity of the mixed solution is reduced and the mixed solution is changed into transparent again, continuously stirring for 0.5-1 h, changing to the vacuum degree of 200Pa, stirring for 20 min at the speed of 100-150 rpm, standing for defoaming in a vacuum state, and filtering on a 100-mesh screen to obtain the composite glass flame-retardant heat-insulating liquid.
5. Use of the composite glass fire-retardant and heat-insulating liquid as defined in any one of claims 1-2 in the production of composite glass.
6. The use according to claim 5, wherein the composite glass is prepared by a method comprising: and (3) pouring the composite glass flame-retardant heat-insulating liquid into a toughened composite glass cavity, wherein the thickness of the cavity is 2-5 mm, the periphery of the composite glass is sealed by an impervious and leakproof single-channel sealant, and the composite glass is obtained after curing for 3-7 h.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5322889A (en) * 1991-09-24 1994-06-21 Mitsubishi Rayon Co., Ltd. Composite composition having high transparency and process for producing same
EP1855878A1 (en) * 2005-03-02 2007-11-21 AGC Flat Glass Europe SA Fireproof glazing
WO2014154969A1 (en) * 2013-03-26 2014-10-02 Saint-Gobain Glass France Fire-resistant glazing
CN105131761A (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

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB0917905D0 (en) * 2009-10-13 2009-11-25 Pilkington Group Ltd Fire resistant glazing
GB201203529D0 (en) * 2012-02-29 2012-04-11 Pilkington Group Ltd Fire resistant glazings

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5322889A (en) * 1991-09-24 1994-06-21 Mitsubishi Rayon Co., Ltd. Composite composition having high transparency and process for producing same
EP1855878A1 (en) * 2005-03-02 2007-11-21 AGC Flat Glass Europe SA Fireproof glazing
WO2014154969A1 (en) * 2013-03-26 2014-10-02 Saint-Gobain Glass France Fire-resistant glazing
CN105131761A (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

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