阅读说明：本技术 一种用有机硅树脂气凝胶填充的防火玻璃及其制作方法 (Fireproof glass filled with organic silicon resin aerogel and manufacturing method thereof ) 是由 何秀冲 王辉林 翁永平 刘杰 于 2021-07-14 设计创作，主要内容包括：本发明公开了一种用有机硅树脂气凝胶填充的防火玻璃及其制作方法。本发明的防火玻璃为在中空的玻璃框架中填充有机硅树脂气凝胶,其中,有机硅树脂气凝胶的配方包括以重量份数计的正硅酸四乙酯8-15份,正硅酸四甲酯10-25份,甲醇5-15份,水20-40份,草酸8-15份,氨水7-50份,正己烷10-25份,有机硅树脂10-30份,胺类固化剂2-15份,以及氢氧化镁5-20份。本发明的有机硅树脂气凝胶配方成分及其制备方法简单,生产过程无有害物质排放,结合本发明的注入工艺,使得本发明的防火玻璃成品无微泡,透光率高,且具有超低的导热系数、良好的耐高低温性能和抗老化性能。(The invention discloses a fireproof glass filled with organic silicon resin aerogel and a manufacturing method thereof. The fireproof glass is prepared by filling organic silicon resin aerogel in a hollow glass frame, wherein the formula of the organic silicon resin aerogel comprises, by weight, 8-15 parts of tetraethyl orthosilicate, 10-25 parts of tetramethyl orthosilicate, 5-15 parts of methanol, 20-40 parts of water, 8-15 parts of oxalic acid, 7-50 parts of ammonia water, 10-25 parts of n-hexane, 10-30 parts of organic silicon resin, 2-15 parts of an amine curing agent and 5-20 parts of magnesium hydroxide. The formula components and the preparation method of the organic silicon resin aerogel are simple, no harmful substance is discharged in the production process, and the injection process is combined, so that the fireproof glass finished product is free of microbubbles, high in light transmittance, ultralow in heat conductivity coefficient, and good in high and low temperature resistance and ageing resistance.)

1. The fireproof glass filled with the organic silicon resin aerogel is characterized in that the organic silicon resin aerogel is filled in a hollow glass frame, and the formula of the organic silicon resin aerogel comprises, by mass, 8-15 parts of tetraethyl orthosilicate, 10-25 parts of tetramethyl orthosilicate, 5-15 parts of methanol, 20-40 parts of water, 8-15 parts of oxalic acid, 7-50 parts of ammonia water, 10-25 parts of n-hexane, 10-30 parts of organic silicon resin, 2-15 parts of an amine curing agent and 5-20 parts of magnesium hydroxide.

2. The fire resistant glass filled with silicone aerogel according to claim 1, wherein said hollow glass frame is made of one or more of tempered glass, cesium potassium glass, microcrystalline glass, borosilicate glass, aluminosilicate glass, float glass, colored glass, coated glass, patterned glass, and laminated glass.

3. The silicone aerogel-filled fire protection glass according to claim 1, wherein the water is deionized water; the mass concentration of the ammonia water is 25%.

4. The fire-resistant glass filled with silicone aerogel according to claim 1, wherein said amine curing agent comprises at least one of aminopropyltrimethoxysilane, aminopropyltriethoxysilane, polyetheramine, aliphatic amine, alicyclic amine, heterocyclic amine and polyamide.

5. The method for manufacturing a fire-proof glass filled with a silicone resin aerogel according to any one of claims 1 to 4, comprising the steps of:

step 1: tetraethyl orthosilicate, tetramethyl orthosilicate, methanol, water and oxalic acid are stirred and mixed uniformly, and then hydrolysis is carried out under the heating condition;

step 2: adding ammonia water for polycondensation reaction to prepare alcogel;

and step 3: placing the alcogel obtained in the step 2 in methanol for aging, and adding n-hexane for reaction to obtain wet gel;

and 4, step 4: stirring the wet gel obtained in the step (3) with organic silicon resin, an amine curing agent and magnesium hydroxide for reaction, and drying the obtained product to obtain the organic silicon resin reinforced heat insulation type silicon dioxide aerogel;

and 5: preparing a hollow glass frame and reserving a grouting opening;

step 6: vacuumizing the silicon dioxide aerogel obtained in the step 4 under the heating condition for defoaming, then injecting the silicon dioxide aerogel subjected to defoaming treatment from a grouting opening, adopting a method of flowing down along the wall of the cup during injection, and standing in a ventilated and cool place for solidification and forming after injection is finished;

and 7: and after the silicon dioxide aerogel is solidified and formed, sealing the grouting opening, and then placing the grouting opening into an oven for treatment so as to sinter and form the silicon dioxide aerogel after thermal phase change solidification, thereby obtaining the finished product of the fireproof glass filled with the organic silicon resin aerogel.

6. The method for manufacturing a fire-proof glass filled with silicone resin aerogel according to claim 5, wherein the hydrolysis conditions in step 1 are as follows: the temperature is 50-60 ℃, and the time is 10-12 h.

7. The method for manufacturing the fireproof glass filled with the silicone resin aerogel according to claim 5, wherein the reaction time in the step 2 is 10-15 hours; and the aging time in the step 3 is 10-15 h.

8. The method for manufacturing the fire-proof glass filled with the silicone resin aerogel according to claim 5, wherein the reaction time in the step 4 is 8-12 hours, and the drying condition is that the glass is dried at 70-80 ℃ for 10-12 hours.

9. The method for manufacturing the fire-proof glass filled with the silicone resin aerogel according to claim 5, wherein the heating temperature in the step 6 is 45-55 ℃, the vacuumizing pressure is less than or equal to 0.01Pa, and the temperature condition for solidification forming is 28-35 ℃.

10. The method for manufacturing a fire-resistant glass filled with silicone aerogel according to claim 5, wherein the conditions of putting into an oven and processing in step 7 are as follows: the temperature is 75-85 ℃, and the time is 10-15 h.

Technical Field

The invention relates to a fireproof glass filled with organic silicon resin aerogel and a manufacturing method thereof, belonging to the technical field of fireproof materials.

Background

Fire prevention work is related to the life of each person of thousands of households, and is one of safe prevention and control important work. Glass can not leave our lives now. Thus, the fireproof glass becomes one of the fireproof materials for our buildings. At present, fireproof glass is also diversified in form. The adopted materials, the process method, the realization effect and the like are different.

The glass is a material with high transparency, strength and hardness and air impermeability, is chemically inert in daily environment and does not react with organisms, so the glass has wide application. In the prior art, glass used for buildings is mainly used for sealing, lighting and heat preservation. With the rapid development of economy in China, the requirements of people on life quality are higher and higher, the area of glass doors and windows of buildings is larger and larger, and the building glass is used as a lighting and decoration material in the past and gradually develops towards the directions of safety fire prevention, heat preservation, heat insulation, sound insulation, noise reduction, intelligent light control and the like.

The aerogel is a light solid material which is formed by stacking nano-scale particles and has nano-scale holes, so that the aerogel has extremely high porosity and specific surface area, excellent chemical stability and incombustibility, and shows excellent light, light transmission, heat insulation, heat preservation, sound insulation, fire prevention and impact resistance. Therefore, if the aerogel and the glass are compounded, the glass door and window simultaneously having the functions of transparency, heat preservation, heat insulation, temperature-sensitive color change and intelligent sun shading can be realized.

Disclosure of Invention

The technical problem solved by the invention is as follows: the technical problem of how to compound aerogel and glass into fireproof glass.

In order to solve the technical problem, the invention provides fireproof glass filled with organic silicon resin aerogel, wherein the fireproof glass is formed by filling the organic silicon resin aerogel in a hollow glass frame, and the formula of the organic silicon resin aerogel comprises, by mass, 8-15 parts of tetraethyl orthosilicate, 10-25 parts of tetramethyl orthosilicate, 5-15 parts of methanol, 20-40 parts of water, 8-15 parts of oxalic acid, 7-50 parts of ammonia water, 10-25 parts of n-hexane, 10-30 parts of organic silicon resin, 2-15 parts of an amine curing agent and 5-20 parts of magnesium hydroxide.

Preferably, the hollow glass frame is made of one or more of tempered glass, cesium potassium glass, microcrystalline glass, borosilicate glass, aluminosilicate glass, float glass, colored glass, coated glass, embossed glass and laminated glass.

Preferably, the water is deionized water; the mass concentration of the ammonia water is 20-30%.

Preferably, the amine curing agent comprises at least one of aminopropyltrimethoxysilane, aminopropyltriethoxysilane, polyetheramine, aliphatic amine, alicyclic amine, heterocyclic amine and polyamide.

The invention also provides a manufacturing method of the fireproof glass filled with the organic silicon resin aerogel, which comprises the following steps:

step 1: tetraethyl orthosilicate, tetramethyl orthosilicate, methanol, water and oxalic acid are stirred and mixed uniformly, and then hydrolysis is carried out under the heating condition;

step 2: adding ammonia water for polycondensation reaction to prepare alcogel;

and step 3: placing the alcogel obtained in the step 2 in methanol for aging, and adding n-hexane for reaction to obtain wet gel;

and 4, step 4: stirring the wet gel obtained in the step (3) with organic silicon resin, an amine curing agent and magnesium hydroxide for reaction, and drying the obtained product to obtain the organic silicon resin reinforced heat insulation type silicon dioxide aerogel;

and 5: preparing a hollow glass frame and reserving a grouting opening;

step 6: vacuumizing the silicon dioxide aerogel obtained in the step 4 under the heating condition for defoaming, then injecting the silicon dioxide aerogel subjected to defoaming treatment from a grouting opening, adopting a method of flowing down along the wall of the cup during injection, and standing in a ventilated and cool place for solidification and forming after injection is finished;

and 7: and after the silicon dioxide aerogel is solidified and formed, sealing the grouting opening, and then placing the grouting opening into an oven for treatment so as to sinter and form the silicon dioxide aerogel after thermal phase change solidification, thereby obtaining the finished product of the fireproof glass filled with the organic silicon resin aerogel.

Preferably, the hydrolysis conditions in step 1 are: the temperature is 50-60 ℃, and the time is 10-12 h;

preferably, the reaction time in the step 2 is 10-15 h; and the aging time in the step 3 is 10-15 h.

Preferably, the reaction time in the step 4 is 8-12 hours, and the drying condition is that the drying is carried out at 70-80 ℃ for 10-12 hours.

Preferably, the heating temperature in the step 6 is 45-55 ℃, the vacuumizing pressure is less than or equal to 0.01Pa, and the solidification forming temperature is 28-35 ℃.

Preferably, the conditions for putting into the oven for treatment in the step 7 are as follows: the temperature is 75-85 ℃, and the time is 10-15 h.

Compared with the prior art, the invention has the following beneficial effects:

1. the formula components and the preparation method of the organic silicon resin aerogel are simple, no harmful substance is discharged in the production process, no solvent is used, and the organic silicon resin aerogel is environment-friendly;

2. when the organic silicon resin aerogel is injected, vacuum defoaming treatment is carried out under a heating condition, no additional defoaming agent is needed, and the fireproof glass prepared by combining the characteristics of the aerogel and the preparation process disclosed by the invention has no micro bubbles and high light transmittance.

Detailed Description

In order to make the invention more comprehensible, preferred embodiments are described in detail below.

Example 1

A method for manufacturing fireproof glass filled with organic silicon resin aerogel comprises the following steps:

1) adding 8 parts of tetraethyl orthosilicate, 12 parts of tetramethyl orthosilicate, 5 parts of methanol, 20 parts of water and 8 parts of oxalic acid into a beaker, stirring for 10 minutes, uniformly mixing, and then placing in a water bath kettle at 50 ℃ for hydrolysis for 10-12 hours;

2) after hydrolysis is finished in the step 1), adding 22 parts of ammonia water solution into a beaker to perform polycondensation reaction to form alcogel;

3) aging the alcogel obtained in the step 2) in methanol for 12 hours, adding 10 parts of n-hexane for reaction, and obtaining wet gel after 12 hours;

4) putting the wet gel obtained in the step 3) and 8 parts of organic silicon resin, 2 parts of methyltrimethoxysilane and 5 parts of magnesium hydroxide into a reactor for reaction for 10 hours, and then drying at 80 ℃ for 10 hours to obtain the organic silicon resin reinforced heat insulation type silicon dioxide aerogel;

5) preparing a hollow glass frame and reserving a grouting opening;

6) preparing a required organic silicon resin aerogel solution according to the volume of the hollow glass frame, heating and stirring the aerogel solution in a heater at 50 ℃, vacuumizing in a vacuum box after 10 minutes, and defoaming when the vacuum requirement reaches minus 0.01 Pa. Then injecting aerogel solution from the grouting opening, adopting a method of 'flowing down along the cup wall' during injection, and standing in a ventilated and cool room at room temperature of about 30 ℃ for solidification and forming after injection.

7) And after solidification and forming, sealing, putting the sealed aerogel into an oven at 80 ℃ for 12 hours to enable the poured aerogel to be sintered and formed after thermal phase change solidification.

Example 2

A method for manufacturing fireproof glass filled with organic silicon resin aerogel comprises the following steps:

1) adding 10 parts of tetraethyl orthosilicate, 10 parts of tetramethyl orthosilicate, 5 parts of methanol, 20 parts of water and 15 parts of oxalic acid into a beaker, stirring for 10 minutes, uniformly mixing, and then placing in a 50 ℃ water bath kettle for hydrolysis for 10-12 hours;

2) after hydrolysis is finished in the step 1), adding 18 parts of ammonia water solution into a beaker to perform polycondensation reaction to form alcogel;

3) aging the alcogel obtained in the step 2) in methanol for 12 hours, adding 10 parts of n-hexane for reaction, and obtaining wet gel after 12 hours;

4) putting the wet gel obtained in the step 3) and 10 parts of organic silicon resin, 2 parts of aminopropyltriethoxysilane and 5 parts of magnesium hydroxide into a reactor for reaction for 10 hours, and then drying at 80 ℃ for 10 hours to obtain the organic silicon resin reinforced heat insulation type silicon dioxide aerogel;

5) preparing a hollow glass frame and reserving a grouting opening;

6) and preparing the required silicone resin aerogel solution according to the volume amount of the hollow glass frame. Then heating the aerogel solution in a heater at 50 ℃ while stirring, vacuumizing in a vacuum box after 10 minutes, and defoaming when the vacuum requirement reaches minus 0.01 Pa. Then injecting aerogel solution from the grouting opening, adopting a method of 'flowing down along the cup wall' during injection, and standing in a ventilated and cool room at room temperature of about 30 ℃ for solidification and forming after injection.

7) And after solidification and forming, sealing, putting the sealed aerogel into an oven at 80 ℃ for 12 hours to enable the poured aerogel to be sintered and formed after thermal phase change solidification.

The performance indexes of the fire-proof glass products filled with the silicone resin aerogel obtained in the above examples 1 and 2 are shown in table 1.

TABLE 1 Performance index of finished fire-resistant glass products obtained in example 1 and example 2

While the invention has been described with respect to a preferred embodiment, 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.