CN102515574B - Preparation method of gel interlayer fireproofing glass - Google Patents

Preparation method of gel interlayer fireproofing glass Download PDF

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Publication number
CN102515574B
CN102515574B CN2011104128049A CN201110412804A CN102515574B CN 102515574 B CN102515574 B CN 102515574B CN 2011104128049 A CN2011104128049 A CN 2011104128049A CN 201110412804 A CN201110412804 A CN 201110412804A CN 102515574 B CN102515574 B CN 102515574B
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gel
glass
agent
distilled water
urea
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CN102515574A (en
Inventor
张长水
姚大虎
吕本莲
杨参
王海棠
沈来喜
沈俊涛
刘静
李平
宋邦才
段文录
柴元武
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Henan University of Science and Technology
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Henan University of Science and Technology
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Abstract

A preparation method of a gel interlayer fireproofing glass comprises the following steps: cleaning cut plate glass, carrying out edge sealing on the glass to prepare interlayer hollow glass and reserving a grouting aperture; and pouring fireproofing transparent gel containing organic gel, crosslinking agent, initiator, ammonium phosphate, magnesium chloride, cane sugar, urea, ethanolamine and distilled water into the hollow glass, sealing the grouting aperture to realize natural cross-linking solidification and obtain a finished product. The fireproofing glass prepared by the invention has a total thickness of 20 mm to reduce weight of the product substantially; and the fireproofing glass has transmittance of 80%, flexibility of 0.1%, UV resistance of 1% and heat tolerance, cold resistance and impact resistance superior to requirements of GB15763.1-2001. The production technology is simple, has high income with low investment, generates no pollution, belongs to green production technology and suits for large-scale popularization.

Description

A kind of preparation method of gel interlayer fireproofing glass
Technical field
The present invention relates to the preparation method of engineering with flame resistant glass, specifically a kind of preparation method of gel interlayer fireproofing glass.
Background technology
Current clip stratotype flame resistant glass is all composite fireproof glass, is divided into water glass filled-type and gel-filled type flame resistant glass.The water-fast weathering resistance of water glass type flame resistant glass is poor, life-time service transparency variation.And the transparency of gel fire-resistance glass is good, water-fast, but while under sunlight long-term irradiation condition, using gel and glassy bond bad, and easily produce bubble, and then affect attractive in appearance and transparent.
Summary of the invention
The objective of the invention is to improve the prior art deficiency, by the composition of organic gel agent and the composition of additive in the change gel, cause transparent variation thereby make the gel interlayer fireproofing glass made under the sunlight long-term irradiation, not be prone to bubble in gel.
The present invention solves the problems of the technologies described above the technical scheme of employing to be: a kind of preparation method of gel interlayer fireproofing glass comprises following operation: the sheet glass of well cutting is cleaned up, then its edge sealing is made to the double glazing of interlayer, and reserved grout hole; The fireproof transparent gel is filled in double glazing and goes by grout hole, and the sealing grout hole, place 48h under 20 ~ 50 ℃ of conditions, makes its natural-crosslinked solidifying, and obtains finished product;
Described fireproof transparent gel is comprised of organic gel agent, linking agent, initiator, ammonium phosphate, magnesium chloride, sucrose, urea, thanomin and distilled water;
Described organic gel agent directly mixes gained by acrylamide and cationic monomer;
In described fireproof transparent gel, the percentage ratio that each component accounts for fireproof transparent gel total mass is respectively: acrylamide 5-20%, cationic monomer 0.5-4%, linking agent 1-10%, initiator 0.5-5%, ammonium phosphate 5-30%, magnesium chloride 5-25%, sucrose 2-20%, urea 3-25%, thanomin 5-30%, all the other are distilled water;
Described cationic monomer is one or more in acrylyl oxy-ethyl-trimethyl salmiac, diallyldimethylammonium chloride, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride or methacrylic dimethylin ethyl ester;
Described linking agent is N,N methylene bis acrylamide;
Described initiator is Potassium Persulphate or ammonium persulphate;
The preparation process of described fireproof transparent gel is:
1) take acrylamide according to the above ratio and cationic monomer is mixed and made into organic gel agent, then organic gel agent is dissolved in distilled water and makes the organogel agent solution, standby;
2) take according to the above ratio respectively linking agent, initiator, ammonium phosphate, magnesium chloride, sucrose, urea and thanomin, linking agent is dissolved in distilled water, after stirring and dissolving, slowly add successively while stirring load weighted ammonium phosphate, magnesium chloride, sucrose, urea and thanomin, Deng after the above-mentioned substance dissolving, add the initiator taken, then continue to stir to obtain clear solution, standby;
3) the organogel agent solution and the step 2 that step 1) are made) clear solution that makes mixes, and stirs 30min, and under the pressure conditions of 50-94kPa, degassed 2h, make the fireproof transparent gel;
Described step 2) in, in process for preparation, solution temperature is controlled within 10 ~ 30 ℃;
In described step 3), during degassed operation, the temperature of solution is controlled at 30-40 ℃.
In order to guarantee the performance of the gel interlayer fireproofing glass that the present invention makes, in described fireproof transparent gel, the percentage ratio that each component accounts for fireproof transparent gel total mass is preferably: acrylamide 8-16%, cationic monomer 1.8-3.2%, linking agent 1-4%, initiator 2-5%, ammonium phosphate 10-25%, magnesium chloride 9-18%, sucrose 4-15%, urea 3-20%, thanomin 5-20%, all the other are distilled water.
In the present invention, organic gel agent is dissolved in distilled water to the step of making the organogel agent solution and linking agent is dissolved in to the step in distilled water, the distilled water added be take and can be dissolved solute and be prerequisite, and the total amount sum of the distilled water added in two steps is the quality of distilled water in the fireproof transparent gel.
In the present invention, the degassed routine operation that is operating as, its objective is and prevent that the fireproof transparent gel from producing bubble when polymerization; After the grouting sealing, be cured polymerization, outside temperature is controlled between 20 ~ 50 ℃, in case too fast gel homogeneity and the transparent variation of causing of polymerization occur.
The product that the present invention makes is through national fire-proof construction material quality supervision and test Spot detection: flame resistant glass total thickness 20mm, the face that catches fire is continuing more than 76 minutes under the high temperature more than 1100 ℃, unexposed surface temperature still can remain on below 130 ℃, category-A II level fire resistance period requirement up to specification; Transparence 80(65) %, sinuousness 0.1(0.3) %, UV resistant irradiation behaviour 1(10) %, thermotolerance, winter hardiness, shock resistance etc. meet the requirements, with similar products at home and abroad, compare, reduced the weight of flame resistant glass unit surface, improve the over-all properties of flame resistant glass, reached domestic and international top standard.
Beneficial effect: 1. the flame resistant glass total thickness of the present invention's production only has 20mm, is less than 30 now current mm, effectively reduces the weight of product;
2. the flame resistant glass of the present invention's production face that catches fire is continuing more than 76 minutes under the high temperature more than 1100 ℃, and unexposed surface temperature still can remain on below 130 ℃, category-A II level fire resistance period requirement up to specification;
3. the flame resistant glass transparence 80(65 that produces of the present invention) %, sinuousness 0.1(0.3) %, UV resistant irradiation behaviour 1(10) %, thermotolerance, winter hardiness, shock resistance etc. be better than GB15763.1-2001Requirement;
4. production technique of the present invention is simple, and the high repayment of low input is pollution-free, belongs to green production process, is suitable for large-scale promotion.
Embodiment
The present invention is further elaborated below in conjunction with specific embodiment.
Embodiment 1
A kind of preparation method of gel interlayer fireproofing glass, first prepare the fireproof transparent gel, the steps include:
1) be mixed and made into organic gel agent by weight taking the acrylamide of 20 parts and the acrylyl oxy-ethyl-trimethyl salmiac of 4 parts respectively, then organic gel agent be dissolved in the distilled water of 16 parts and make the organogel agent solution, standby;
2) by weight taking respectively the N of 10 parts, N-methylene-bisacrylamide, the Potassium Persulphate of 0.5 part, the ammonium phosphate of 5 parts, the magnesium chloride of 5 parts, the sucrose of 11 parts, the urea of 3 parts and the thanomin of 5 parts, by load weighted N, the N-methylene-bisacrylamide is dissolved in the distilled water of 20.5 parts, after stirring and dissolving, slowly add successively while stirring load weighted ammonium phosphate, magnesium chloride, sucrose, urea and thanomin, Deng it, thoroughly after dissolving, add the Potassium Persulphate taken, then continue to stir to obtain clear solution, standby;
3) the organogel agent solution and the step 2 that step 1) are made) clear solution that makes mixes, and stirs 30min, and under the pressure of 94kPa, degassed 2h, make the fireproof transparent gel.
Then the sheet glass of well cutting is cleaned up, then its edge sealing is made to the double glazing of interlayer, and reserved grout hole; The fireproof transparent gel prepared is filled in double glazing and goes by grout hole, and the sealing grout hole, place 48h under 20 ℃ of conditions, makes its natural-crosslinked solidifying, and obtains finished product.
Embodiment 2
A kind of preparation method of gel interlayer fireproofing glass, first prepare the fireproof transparent gel, the steps include:
1) be mixed and made into organic gel agent by weight taking the acrylamide of 5 parts and the diallyldimethylammonium chloride of 0.5 part respectively, then organic gel agent be dissolved in the distilled water of 4 parts and make the organogel agent solution, standby;
2) by weight taking respectively the N of 1 part, N-methylene-bisacrylamide, the Potassium Persulphate of 5 parts, the ammonium phosphate of 30 parts, the magnesium chloride of 5 parts, the sucrose of 2 parts, the urea of 3 parts and the thanomin of 17 parts, by load weighted N, the N-methylene-bisacrylamide is dissolved in the distilled water of 27.5 parts, after stirring and dissolving, slowly add successively while stirring load weighted ammonium phosphate, magnesium chloride, sucrose, urea and thanomin, Deng it, thoroughly after dissolving, add the Potassium Persulphate taken, then continue to stir to obtain clear solution, standby;
3) the organogel agent solution and the step 2 that step 1) are made) clear solution that makes mixes, and stirs 30min, and under the pressure of 50kPa, degassed 2h, make the fireproof transparent gel.
Then the sheet glass of well cutting is cleaned up, then its edge sealing is made to the double glazing of interlayer, and reserved grout hole; The fireproof transparent gel prepared is filled in double glazing and goes by grout hole, and the sealing grout hole, place 48h under 50 ℃ of conditions, makes its natural-crosslinked solidifying, and obtains finished product.
Embodiment 3
A kind of preparation method of gel interlayer fireproofing glass, first prepare the fireproof transparent gel, the steps include:
1) be mixed and made into organic gel agent by weight taking the acrylamide of 12 parts and the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride of 2 parts respectively, then organic gel agent be dissolved in the distilled water of 9 parts and make the organogel agent solution, standby;
2) by weight taking respectively the N of 5 parts, N-methylene-bisacrylamide, the ammonium persulphate of 3 parts, the ammonium phosphate of 5 parts, the magnesium chloride of 25 parts, the sucrose of 2 parts, the urea of 3 parts and the thanomin of 5 parts, by load weighted N, the N-methylene-bisacrylamide is dissolved in the distilled water of 29 parts, after stirring and dissolving, slowly add successively while stirring load weighted ammonium phosphate, magnesium chloride, sucrose, urea and thanomin, Deng it, thoroughly after dissolving, add the ammonium persulphate taken, then continue to stir to obtain clear solution, standby;
3) the organogel agent solution and the step 2 that step 1) are made) clear solution that makes mixes, and stirs 30min, and under the pressure of 70kPa, degassed 2h, make the fireproof transparent gel.
Then the sheet glass of well cutting is cleaned up, then its edge sealing is made to the double glazing of interlayer, and reserved grout hole; The fireproof transparent gel prepared is filled in double glazing and goes by grout hole, and the sealing grout hole, place 48h under 35 ℃ of conditions, makes its natural-crosslinked solidifying, and obtains finished product.
Embodiment 4
A kind of preparation method of gel interlayer fireproofing glass, first prepare the fireproof transparent gel, the steps include:
1) be mixed and made into organic gel agent by weight taking the acrylamide of 5 parts and the methacrylic dimethylin ethyl ester of 0.5 part respectively, then organic gel agent be dissolved in the distilled water of 4 parts and make the organogel agent solution, standby;
2) by weight taking respectively the N of 1 part, N-methylene-bisacrylamide, the ammonium persulphate of 0.5 part, the ammonium phosphate of 5 parts, the magnesium chloride of 15 parts, the sucrose of 2 parts, the urea of 25 parts and the thanomin of 5 parts, by load weighted N, the N-methylene-bisacrylamide is dissolved in the distilled water of 37 parts, after stirring and dissolving, slowly add successively while stirring load weighted ammonium phosphate, magnesium chloride, sucrose, urea and thanomin, Deng it, thoroughly after dissolving, add the ammonium persulphate taken, then continue to stir to obtain clear solution, standby;
3) the organogel agent solution and the step 2 that step 1) are made) clear solution that makes mixes, and stirs 30min, and under the pressure of 80kPa, degassed 2h, make the fireproof transparent gel.
Then the sheet glass of well cutting is cleaned up, then its edge sealing is made to the double glazing of interlayer, and reserved grout hole; The fireproof transparent gel prepared is filled in double glazing and goes by grout hole, and the sealing grout hole, place 48h under 40 ℃ of conditions, makes its natural-crosslinked solidifying, and obtains finished product.
Embodiment 5
A kind of preparation method of gel interlayer fireproofing glass, first prepare the fireproof transparent gel, the steps include:
1) be mixed and made into organic gel agent by weight taking the acrylamide of 5 parts and the methacrylic dimethylin ethyl ester of 2 parts respectively, then organic gel agent be dissolved in the distilled water of 4.5 parts and make the organogel agent solution, standby;
2) by weight taking respectively the N of 5 parts, N-methylene-bisacrylamide, the Potassium Persulphate of 3 parts, the ammonium phosphate of 17 parts, the magnesium chloride of 5 parts, the sucrose of 20 parts, the urea of 3 parts and the thanomin of 5 parts, by load weighted N, the N-methylene-bisacrylamide is dissolved in the distilled water of 30.5 parts, after stirring and dissolving, slowly add successively while stirring load weighted ammonium phosphate, magnesium chloride, sucrose, urea and thanomin, Deng it, thoroughly after dissolving, add the Potassium Persulphate taken, then continue to stir to obtain clear solution, standby;
3) the organogel agent solution and the step 2 that step 1) are made) clear solution that makes mixes, and stirs 30min, and under the pressure of 60kPa, degassed 2h, make the fireproof transparent gel.
Then the sheet glass of well cutting is cleaned up, then its edge sealing is made to the double glazing of interlayer, and reserved grout hole; The fireproof transparent gel prepared is filled in double glazing and goes by grout hole, and the sealing grout hole, place 48h under 25 ℃ of conditions, makes its natural-crosslinked solidifying, and obtains finished product.
Embodiment 6
A kind of preparation method of gel interlayer fireproofing glass, first prepare the fireproof transparent gel, the steps include:
1) be mixed and made into organic gel agent by weight taking the acrylamide of 5 parts and the acrylyl oxy-ethyl-trimethyl salmiac of 0.5 part respectively, then organic gel agent be dissolved in the distilled water of 4 parts and make the organogel agent solution, standby;
2) by weight taking respectively the N of 1 part, N-methylene-bisacrylamide, the ammonium persulphate of 0.5 part, the ammonium phosphate of 5 parts, the magnesium chloride of 5 parts, the sucrose of 2 parts, the urea of 14 parts and the thanomin of 30 parts, by load weighted N, the N-methylene-bisacrylamide is dissolved in the distilled water of 33 parts, after stirring and dissolving, slowly add successively while stirring load weighted ammonium phosphate, magnesium chloride, sucrose, urea and thanomin, Deng it, thoroughly after dissolving, add the ammonium persulphate taken, then continue to stir to obtain clear solution, standby;
3) the organogel agent solution and the step 2 that step 1) are made) clear solution that makes mixes, and stirs 30min, and under the pressure of 55kPa, degassed 2h, make the fireproof transparent gel.
Then the sheet glass of well cutting is cleaned up, then its edge sealing is made to the double glazing of interlayer, and reserved grout hole; The fireproof transparent gel prepared is filled in double glazing and goes by grout hole, and the sealing grout hole, place 48h under 30 ℃ of conditions, makes its natural-crosslinked solidifying, and obtains finished product.
The above-mentioned product made is through national fire-proof construction material quality supervision and test Spot detection: flame resistant glass total thickness 20mm, the face that catches fire is continuing more than 76 minutes under the high temperature more than 1100 ℃, unexposed surface temperature still can remain on below 130 ℃, category-A II level fire resistance period requirement up to specification; Transparence 80(65) %; Sinuousness 0.1(0.3) %, UV resistant irradiation behaviour 1(10) %, thermotolerance, winter hardiness, shock resistance etc. meet the requirements.

Claims (2)

1. the preparation method of a gel interlayer fireproofing glass, is characterized in that, comprises following operation: the sheet glass of well cutting is cleaned up, then its edge sealing is made to the double glazing of interlayer, and reserved grout hole; The fireproof transparent gel is filled in double glazing and goes by grout hole, and the sealing grout hole, place 48h under 20 ~ 50 ℃ of conditions, makes its natural-crosslinked solidifying, and obtains finished product;
Described fireproof transparent gel is comprised of organic gel agent, linking agent, initiator, ammonium phosphate, magnesium chloride, sucrose, urea, thanomin and distilled water;
Described organic gel agent directly mixes gained by acrylamide and cationic monomer;
In described fireproof transparent gel, the percentage ratio that each component accounts for fireproof transparent gel total mass is respectively: acrylamide 5-20%, cationic monomer 0.5-4%, linking agent 1-10%, initiator 0.5-5%, ammonium phosphate 5-30%, magnesium chloride 5-25%, sucrose 2-20%, urea 3-25%, thanomin 5-30%, all the other are distilled water;
Described cationic monomer is one or more in acrylyl oxy-ethyl-trimethyl salmiac, diallyldimethylammonium chloride, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride or methacrylic dimethylin ethyl ester;
Described linking agent is N,N methylene bis acrylamide;
Described initiator is Potassium Persulphate or ammonium persulphate;
The preparation process of described fireproof transparent gel is:
1) take acrylamide according to the above ratio and cationic monomer is mixed and made into organic gel agent, then organic gel agent is dissolved in distilled water and makes the organogel agent solution, standby;
2) take according to the above ratio respectively linking agent, initiator, ammonium phosphate, magnesium chloride, sucrose, urea and thanomin, linking agent is dissolved in distilled water, after stirring and dissolving, slowly add successively while stirring load weighted ammonium phosphate, magnesium chloride, sucrose, urea and thanomin, Deng after the above-mentioned substance dissolving, add the initiator taken, then continue to stir to obtain clear solution, standby;
3) the organogel agent solution and the step 2 that step 1) are made) clear solution that makes mixes, and stirs 30min, and under the pressure conditions of 50-94kPa, degassed 2h, make the fireproof transparent gel;
Described step 2) in, in process for preparation, solution temperature is controlled within 10 ~ 30 ℃;
In described step 3), during degassed operation, the temperature of solution is controlled at 30-40 ℃.
2. the preparation method of a kind of gel interlayer fireproofing glass according to claim 1, it is characterized by: in described fireproof transparent gel, the percentage ratio that each component accounts for fireproof transparent gel total mass is respectively: acrylamide 8-16%, cationic monomer 1.8-3.2%, linking agent 1-4%, initiator 2-5%, ammonium phosphate 10-25%, magnesium chloride 9-18%, sucrose 4-15%, urea 3-20%, thanomin 5-20%, all the other are distilled water.
CN2011104128049A 2011-12-13 2011-12-13 Preparation method of gel interlayer fireproofing glass Expired - Fee Related CN102515574B (en)

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US10576424B2 (en) 2013-09-17 2020-03-03 Bl Technologies, Inc. Ion exchange polymers and a method for making ion exchange polymers
CN106145699A (en) * 2016-06-27 2016-11-23 蚌埠市鑫民玻璃有限公司 The composite fireproof glass that a kind of heat-proof quality is good
CN106145702A (en) * 2016-06-27 2016-11-23 蚌埠市鑫民玻璃有限公司 A kind of composite fireproof glass
CN106142764A (en) * 2016-06-27 2016-11-23 蚌埠市鑫民玻璃有限公司 The interlayer fireproofing glass that a kind of light transmission is good
CN106084124A (en) * 2016-06-27 2016-11-09 蚌埠市鑫民玻璃有限公司 A kind of fire retardant for high printing opacity interlayer fireproofing glass and preparation method thereof
CN110330240A (en) * 2019-07-09 2019-10-15 河南恒鑫丰安防科技有限责任公司 A kind of composite fireproof glass colorless transparent gel material and preparation method thereof
CN111518488A (en) * 2020-04-24 2020-08-11 金慧材料(杭州)有限公司 Anti-yellowing fireproof liquid, preparation method thereof, fireproof glass and glass glue filling process

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CN1408665A (en) * 2001-09-26 2003-04-09 舱壁玻璃公司 Fire-proof glass constructed by glass plate and gel layer in laminated layer mode
CN1583640A (en) * 2004-06-01 2005-02-23 姚贞香 Grouting fireproof glass and transparent fireproof gel in it

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