CN105835512B - A kind of preparation method of no microvesicle radioresistance grouting-type flame resistant glass - Google Patents
A kind of preparation method of no microvesicle radioresistance grouting-type flame resistant glass Download PDFInfo
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- CN105835512B CN105835512B CN201610176134.8A CN201610176134A CN105835512B CN 105835512 B CN105835512 B CN 105835512B CN 201610176134 A CN201610176134 A CN 201610176134A CN 105835512 B CN105835512 B CN 105835512B
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- 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
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
- B32B37/1284—Application of adhesive
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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
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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
- 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
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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
- 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
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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
- 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
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
- B32B2037/1269—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives multi-component adhesive
-
- 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
-
- 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
-
- 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
- B32B2307/70—Other properties
- B32B2307/71—Resistive to light or to UV
Abstract
A kind of preparation method of no microvesicle radioresistance grouting-type flame resistant glass is that polyalcohol, surfactant, preservative are added in Ludox and stirred evenly, dimethyl silicone polymer and 2 alkylols are uniformly mixed obtained Compounded Antifoamer again, and it is added into mix silica sol and vacuumizes stirring, the Ludox dispersion liquid of stable and uniform is made, KOH dilutions are added in Ludox dispersion liquid and stirred evenly again, glue then is circulated into the curing of laminated glass high temperature obtains grouting-type flame resistant glass.This method is done antifoaming agent and is cured using isopropanol and dimethyl silicone polymer compounding, the light transmittance of flame resistant glass reaches 86.6%, light transmittance variation is 5.8% after ultraviolet light irradiation, and bubble is few, effectively improve it is traditional using polyacrylamide as the weatherability difference of the grouting-type flame resistant glass of squeegee and more bubble the phenomenon that.
Description
Technical field
The present invention relates to a kind of preparation method of flame resistant glass, especially a kind of no microvesicle radioresistance grouting-type flame resistant glass
Preparation method.
Background technology
Usually by more than two layers original sheet glass, surrounding is sealed grouting-type flame resistant glass with flame-retardant rubber strip, centre perfusion fire prevention
Glue is formed.Traditional fire prevention glue adds initiator, coupling agent and other helps mainly based on acrylamides
Agent.Use and acrylamide itself due to coupling agent is the reason of organic matter, can be brought bubble to glass product, fission,
Whiten, the defects of UV resistant performance is poor, seriously affect its performance.
CN104513032A is disclosed " a kind of flame resistant glass is formulated with clear gel ".Its each component accounts for gross mass hundred
Score is respectively：Ethanol amine 4-25%, initiator 0.1-3%, magnesium chloride 5-20%, gelling agent 5-20%, ammonium phosphate 5-20%, urea
2-30%, boric acid 1-15%, sodium chloride 2-20%, surplus are water.Gelling agent mainly has acrylamide and vinyl alcohol, which makees
Flame resistant glass UV resistant performance is caused to weaken for primary raw material, easily aging；The inorganic salts such as ammonium phosphate, boric acid, sodium chloride
It is a large amount of to add in the light transmittance for affecting flame resistant glass and bubble is generated in whipping process, while do not contain and disappear in the formula
Infusion also results in the generation of bubble in whipping process, and the use of initiator can also make gelling agent generate gas in cross-linking process
Bubble.
CN102515574A is disclosed " a kind of preparation method of gel interlayer fireproofing glass ".The transparent of the flame resistant glass is prevented
Fiery gel mainly includes machine gelling agent acrylamide, crosslinking agent, initiator, ammonium phosphate, magnesium chloride, sucrose, urea element, ethanol amine
And distilled water.Acrylamide is primary raw material, but can weaken the UV resistant performance of flame resistant glass as organic matter；Crosslinking
Agent and initiator can generate a large amount of bubbles in organic polymer whipping process；Ammonium phosphate, magnesium chloride, sucrose, urea element and ethyl alcohol
The a large amount of of amine use the light transmittance for having seriously affected glass.
KR2011136705A is disclosed " a kind of resin Composition of flame resistant glass ".Its primary raw material include Ludox,
KOH, boric acid and stabilizer.Ludox and KOH can significantly improve the UV resistant irradiation property of flame resistant glass as primary raw material；
But the component does not have the use of antifoaming agent, therefore inevitably brings a large amount of bubbles to flame resistant glass；The patent does not have
Light transmittance, UV resistant irradiation performance are detected.
Invention content
The invention solves concrete technical problems be glass raw material that performance is selected to stablize, prepare suitable compounding defoaming
Agent and heat safe fire prevention slurry, and a kind of preparation method of no microvesicle radioresistance grouting-type flame resistant glass is provided.
In order to achieve the above object, the technical solution adopted in the present invention is as follows：
A kind of preparation method of no microvesicle radioresistance grouting-type flame resistant glass is pressed by raw material composition and its mass parts content
Row step carries out：
（1）By 60 ~ 80 parts of Ludox, 10 ~ 15 parts of polyalcohol, 1 ~ 3 part of surfactant, 1-2 parts of preservative
It adds in three-necked flask, temperature is 60 DEG C, heating water bath stirs 1h under rotating speed 20r/s.
（2）It is 1 in mass ratio:1 weighs dimethyl silicone polymer and 2- alkylols, is stirred evenly at normal temperatures with glass bar
Obtain Compounded Antifoamer.
（3）By above-mentioned steps（2）Compounded Antifoamer add in above-mentioned steps（1）Mix silica sol in, temperature be 60
DEG C, rotating speed to stir 10min under 15r/s, be then evacuated to 0.05MPa, and be stirred under vacuum 10min, obtain stable and uniform
Ludox dispersion liquid.
（4）10-17 parts of KOH are taken, a concentration of 50% solution is made, is slowly added to above-mentioned steps（3）In Ludox
In dispersion liquid, temperature for 60 DEG C, mixing speed 50min is stirred under 30r/s, then stir 10min under 0.05MPa, connect
It and is cooled to 30 DEG C, low whipping speed is to stir 30min under 10r/s, obtains fire prevention glue.
（5）Deionized water is filled into preprepared double layer glass cavity, is placed in 1h in 80 DEG C of drying box, so
Afterwards by glass taking-up ultrasonic cleaning 1h, then with deionized water carry out secondary cleaning；Again by above-mentioned steps（4）In fireproof gum
Liquid is slowly fed into glass cavity, during which gently taps glass with mallet, to ensure that bubble is discharged, by the mouth silicon that is in the milk after filling
Ketone glass cement is closed, and glass is placed in 80 DEG C of air dry oven, places 12h, is cured fire prevention glue, that is, is prepared into anti-spoke
Penetrate grouting-type flame resistant glass.
Further, the preparation method is to follow these steps to carry out by raw material composition and its mass parts content：
（1）By 70 part 50% of Ludox, 15 parts of polyalcohols, 2 parts of surfactants, 2 parts three mouthfuls of burnings of preservative addition
In bottle, in the case where temperature is 60 DEG C, rotating speed is 20r/s, heating water bath stirs 1h.
（2）By 1:1 weighs dimethyl silicone polymer and 2- alkylols, is stirred evenly compounded with glass bar at normal temperatures
Antifoaming agent.
（3）By above-mentioned steps（2）Compounded Antifoamer add in above-mentioned steps（1）Mix silica sol in, temperature be 60
DEG C, rotating speed to stir 10min under 15r/s, be then evacuated to 0.05MPa, and vacuumize stirring 10min, obtain stable and uniform
Ludox dispersion liquid.
（4）15 parts of KOH is taken, a concentration of 50% solution is made, is slowly added to above-mentioned steps（3）Ludox point
It it is 60 DEG C in temperature, mixing speed stirs 50min under 30r/s, 10min is then stirred under 0.05MPa, then in dispersion liquid
30 DEG C are cooled to, then low whipping speed obtains fire prevention glue to stir 30min under 10r/s.
（5）Deionized water is filled into preprepared double layer glass cavity, is placed in 1h in 80 DEG C of drying box, so
Afterwards by glass taking-up ultrasonic cleaning 1h, then with deionized water carry out secondary cleaning；By above-mentioned steps（4）In fire prevention glue
It is slowly fed into glass cavity, during which gently taps glass with mallet, so that bubble is discharged, will be filled with silicone glass cement after filling
Mouth closing is starched, glass is placed in 80 DEG C of air dry oven, places 12h, fire prevention glue is allowed to cure, obtains the anti-spoke of no microvesicle
Penetrate grouting-type flame resistant glass.
Additional technical feature in the above-mentioned technical solutions is as follows.
The Ludox is alkaline silica sol, content 50%, grain size 100nm.
The polyalcohol be ethylene glycol, glycerine, two polyethylene glycol, propylene glycol and one kind in two polypropylene glycols or it
Combination.
The surfactant is dimethyl silicone polymer, glycerin monostearate, fatty acid sorbitan and polysorbate
In one kind or combination thereof.
It is one kind or combination thereof in tin oxide, phosphorous oxide, zinc oxide and borax that the preservative, which is,.
The 2- alkylols are isopropanol, 2- butanol, one kind or combination thereof in 2- amylalcohols.
The total addition level of the Compounded Antifoamer is 4 parts, and wherein Compounded Antifoamer is by isopropanol and polydimethylsiloxanes
Alkane forms, and mass ratio is 1:1.
The preparation method is to do antifoaming agent by isopropanol and dimethyl silicone polymer compounding, is cured with KOH, when
SiO2It is 9 in molar ratio with KOH:When 4, flame resistant glass light transmittance obtained is 86.6%.
Implement the preparation method of a kind of no microvesicle radioresistance grouting-type flame resistant glass that the invention described above is provided, using silicon
Colloidal sol and KOH raw materials, further improve ultra-violet radiation resisting and high temperature resistant；It is compounded using isopropanol and dimethyl silicone polymer
As antifoaming agent, it is suppressed that the generation of bubble, and cured with KOH, realize a kind of light transmittance height, ultra-violet radiation resisting
By force, heat safe method for glass preparation.
In said program of the present invention, work as SiO2Ratio with KOH is 9:It when 4, is provided according to GB15763.1, using can
See light thoroughly/reflectance test instrument, resistance to irradiation box and repacking Muffle furnace to the light transmittance of flame resistant glass, UV resistant performance and Nai Gao
Warm nature can be detected, and 86.6% is up to through measuring flame resistant glass light transmittance, and light transmittance variation is 5.8% after ultraviolet light irradiation,
Fire resistance period reaches 90min, effectively improves traditional using polyacrylamide as the resistance to of the grouting-type flame resistant glass of squeegee
The phenomenon that time property difference and more bubble.
Description of the drawings
Fig. 1 is the stereoscopic schematic diagram without microvesicle radioresistance grouting-type flame resistant glass made from this method.In figure：1 and 2 be two
The sheet glass on side；3 be flame retardant sealant item.
Fig. 2 is the flame resistant glass pictorial diagram for not adding in antifoaming agent.
Fig. 3 is the flame resistant glass pictorial diagram that method adds in antifoaming agent.
Specific embodiment
The specific embodiment of the present invention is further illustrated below.
Implement a kind of preparation method of no microvesicle radioresistance grouting-type flame resistant glass, the constituent of this method fire prevention glue
Including alkaline silica sol, Compounded Antifoamer, polyalcohol, surfactant, preservative, deionized water.Wherein alkaline silica sol
SiO2Content is 50%, grain size 100nm；The polyalcohol is ethylene glycol, glycerine, two polyethylene glycol, propylene glycol and dimerization third
One kind or combination thereof in glycol；The surfactant is dimethyl silicone polymer, glycerin monostearate, aliphatic acid
The smooth one kind or combination thereof in polysorbate of sorb；The preservative is in tin oxide, phosphorous oxide, zinc oxide and borax
One kind or combination thereof；The 2- alkylols are isopropanol, 2- butanol, one kind or combination thereof in 2- amylalcohols；
The Compounded Antifoamer is 1 in mass ratio by isopropanol and dimethyl silicone polymer:1 is made.Slurry agitation is uniform, and add
Enter a concentration of 50% KOH solution, work as SiO2Molar ratio with KOH is 9:When 4, flame resistant glass light transmittance obtained reaches
86.6%, light transmittance variation is 5.8% after ultraviolet light irradiates 100 hours, and flame resistant glass bubble is few, effectively improves traditional
Using polyacrylamide as the grouting-type flame resistant glass weatherability of squeegee is poor, the situation more than bubble.Specific embodiment is as follows.
(1) by 60 ~ 80 parts of Ludox, 10 ~ 15 parts of polyalcohol, 1 ~ 3 part of surfactant, 1-2 parts of anti-corrosion
Agent is added in three-necked flask, temperature is 60 DEG C, heating water bath stirs 1h under rotating speed 20r/s；
（2）It is 1 in mass ratio:1 weighs dimethyl silicone polymer and 2- alkylols, is stirred evenly at normal temperatures with glass bar
Obtain Compounded Antifoamer.
（3）By above-mentioned steps（2）3 ~ 6 parts of Compounded Antifoamer addition above-mentioned steps（1）Mix silica sol in, in temperature
10min is stirred under being 15r/s for 60 DEG C, rotating speed, is then evacuated to 0.05MPa, and be stirred under vacuum 10min, obtains and stablizes
Even Ludox dispersion liquid.
（4）10 ~ 17 parts of KOH are taken, a concentration of 50% solution is made, is slowly added to above-mentioned steps（3）In Ludox
In dispersion liquid, temperature for 60 DEG C, mixing speed 50min is stirred under 30r/s, then stir 10min under 0.05MPa, connect
It and is cooled to 30 DEG C, low whipping speed is to stir 30min under 10r/s, obtains fire prevention glue.
（5）Deionized water is filled into preprepared double layer glass cavity, is placed in 1h in 80 DEG C of drying box, so
Afterwards by glass taking-up ultrasonic cleaning 1h, then with deionized water carry out secondary cleaning；Again by above-mentioned steps（4）In fireproof gum
Liquid is slowly fed into glass cavity, during which gently taps glass with mallet, to ensure that bubble is discharged, by the mouth silicon that is in the milk after filling
Ketone glass cement is closed, and glass is placed in 80 DEG C of air dry oven, places 12h, is cured fire prevention glue, that is, is prepared into anti-spoke
Penetrate grouting-type flame resistant glass.According to GB15763.1-2001《Safety glass flame resistant glass for building》Test the saturating of flame resistant glass
Light rate and UV resistant performance, and the outer air bubble problem of flame resistant glass is observed, it is resistance to then will to characterize its in glass merging Muffle furnace
Fire screen is hot.
The specific embodiment of the present invention further illustrated by following embodiment, and that the present invention is not restricted to these is real
Apply example.
Embodiment 1
(1) by 70 parts of Ludox, 10 parts of polyalcohol, 1 part of surfactant, 1 part three mouthfuls of burnings of preservative addition
In bottle, temperature is 60 DEG C, heating water bath stirs 1h under rotating speed 20r/s.
（2）It is 1 in mass ratio:1 weighs dimethyl silicone polymer and 2- alkylols, is stirred evenly at normal temperatures with glass bar
Obtain Compounded Antifoamer.
（3）By above-mentioned steps（2）Compounded Antifoamer add in above-mentioned steps（1）Mix silica sol in, temperature be 60
DEG C, rotating speed to stir 10min under 15r/s, be then evacuated to 0.05MPa, and be stirred under vacuum 10min, obtain stable and uniform
Ludox dispersion liquid.
（4）15 parts of KOH are taken, a concentration of 50% solution is made, is slowly added to above-mentioned steps（3）In Ludox point
In dispersion liquid, temperature for 60 DEG C, mixing speed 50min is stirred under 30r/s, 10min is then stirred under 0.05MPa, then
30 DEG C are cooled to, low whipping speed is to stir 30min under 10r/s, obtains fire prevention glue.
（5）Deionized water is filled into preprepared double layer glass cavity, is placed in 1h in 80 DEG C of drying box, so
Afterwards by glass taking-up ultrasonic cleaning 1h, then with deionized water carry out secondary cleaning；Again by above-mentioned steps（4）In fireproof gum
Liquid is slowly fed into glass cavity, during which gently taps glass with mallet, to ensure that bubble is discharged, by the mouth silicon that is in the milk after filling
Ketone glass cement is closed, and glass is placed in 80 DEG C of air dry oven, places 12h, is cured fire prevention glue, that is, is prepared into anti-spoke
Penetrate grouting-type flame resistant glass.According to GB15763.1-2001《Safety glass flame resistant glass for building》Test the saturating of flame resistant glass
Light rate and UV resistant performance, and the outer air bubble problem of flame resistant glass is observed, it is resistance to then will to characterize its in glass merging Muffle furnace
Fire screen is hot.
The flame resistant glass light transmittance 86.5 of gained, after ultraviolet light irradiates, light transmittance variation is 5.5%, and microvesicle is few, and
And fire resistance period reaches 100min.
Embodiment 2
(1) by 70 parts of Ludox, 11 parts of polyalcohol, 2 parts of surfactant, 2 parts of three mouthfuls of preservative addition
In flask, temperature is 60 DEG C, heating water bath stirs 1h under rotating speed 20r/s.
（2）It is 1 in mass ratio:1 weighs dimethyl silicone polymer and 2- alkylols, is stirred evenly at normal temperatures with glass bar
Obtain Compounded Antifoamer.
（3）By above-mentioned steps（2）Compounded Antifoamer add in above-mentioned steps（1）Mix silica sol in, temperature be 60
DEG C, rotating speed to stir 15min under 15r/s, be then evacuated to 0.05MPa, and be stirred under vacuum 15min, obtain stable and uniform
Ludox dispersion liquid.
（4）15 parts of KOH are taken, a concentration of 50% solution is made, is slowly added to above-mentioned steps（3）In Ludox point
In dispersion liquid, temperature for 60 DEG C, mixing speed 50min is stirred under 30r/s, 10min is then stirred under 0.05MPa, then
30 DEG C are cooled to, low whipping speed is to stir 30min under 10r/s, obtains fire prevention glue.
（5）Deionized water is filled into preprepared double layer glass cavity, is placed in 1h in 80 DEG C of drying box, so
Afterwards by glass taking-up ultrasonic cleaning 1h, then with deionized water carry out secondary cleaning；Again by above-mentioned steps（4）In fireproof gum
Liquid is slowly fed into glass cavity, during which gently taps glass with mallet, to ensure that bubble is discharged, by the mouth silicon that is in the milk after filling
Ketone glass cement is closed, and glass is placed in 80 DEG C of air dry oven, places 12h, is cured fire prevention glue, that is, is prepared into anti-spoke
Penetrate grouting-type flame resistant glass.According to GB15763.1-2001《Safety glass flame resistant glass for building》Test the saturating of flame resistant glass
Light rate and UV resistant performance, and the outer air bubble problem of flame resistant glass is observed, it is resistance to then will to characterize its in glass merging Muffle furnace
Fire screen is hot.
The flame resistant glass light transmittance 86.7 of gained, after ultraviolet light irradiates, light transmittance variation is 5.8%, and microvesicle is few, and
And fire resistance period reaches 110min.
Embodiment 3
(1) by 70 parts of Ludox, 12 parts of polyalcohol, 3 parts of surfactant, 3 parts three mouthfuls of burnings of preservative addition
In bottle, temperature is 60 DEG C, heating water bath stirs 1h under rotating speed 20r/s.
（2）It is 1 in mass ratio:1 weighs dimethyl silicone polymer and 2- alkylols, is stirred evenly at normal temperatures with glass bar
Obtain Compounded Antifoamer.
（3）By above-mentioned steps（2）Compounded Antifoamer add in above-mentioned steps（1）Mix silica sol in, temperature be 60
DEG C, rotating speed to stir 15min under 20r/s, be then evacuated to 0.05MPa, and be stirred under vacuum 15min, obtain stable and uniform
Ludox dispersion liquid.
（4）15 parts of KOH are taken, a concentration of 50% solution is made, is slowly added to above-mentioned steps（3）In Ludox point
In dispersion liquid, temperature for 60 DEG C, mixing speed 50min is stirred under 30r/s, 10min is then stirred under 0.05MPa, then
30 DEG C are cooled to, low whipping speed is to stir 30min under 10r/s, obtains fire prevention glue.
（5）Deionized water is filled into preprepared double layer glass cavity, is placed in 1h in 80 DEG C of drying box, so
Afterwards by glass taking-up ultrasonic cleaning 1h, then with deionized water carry out secondary cleaning；Again by above-mentioned steps（4）In fireproof gum
Liquid is slowly fed into glass cavity, during which gently taps glass with mallet, to ensure that bubble is discharged, by the mouth silicon that is in the milk after filling
Ketone glass cement is closed, and glass is placed in 80 DEG C of air dry oven, places 15h, is cured fire prevention glue, that is, is prepared into anti-spoke
Penetrate grouting-type flame resistant glass.According to GB15763.1-2001《Safety glass flame resistant glass for building》Test the saturating of flame resistant glass
Light rate and UV resistant performance, and the outer air bubble problem of flame resistant glass is observed, it is resistance to then will to characterize its in glass merging Muffle furnace
Fire screen is hot.
The flame resistant glass light transmittance 86.3 of gained, after ultraviolet light irradiates, light transmittance variation is 5.4%, and microvesicle is few, and
And fire resistance period reaches 107min.
Embodiment 4
(1) by 70 parts of Ludox, 13 parts of polyalcohol, 3 parts of surfactant, 3 parts three mouthfuls of burnings of preservative addition
In bottle, temperature is 60 DEG C, heating water bath stirs 1h under rotating speed 20r/s.
（2）It is 1 in mass ratio:1 weighs dimethyl silicone polymer and 2- alkylols, is stirred evenly at normal temperatures with glass bar
Obtain Compounded Antifoamer.
（3）By above-mentioned steps（2）Compounded Antifoamer add in above-mentioned steps（1）Mix silica sol in, temperature be 60
DEG C, rotating speed to stir 15min under 20r/s, be then evacuated to 0.05MPa, and be stirred under vacuum 15min, obtain stable and uniform
Ludox dispersion liquid.
（4）15 parts of KOH are taken, a concentration of 50% solution is made, is slowly added to above-mentioned steps（3）In Ludox point
In dispersion liquid, temperature for 60 DEG C, mixing speed 50min is stirred under 30r/s, 10min is then stirred under 0.05MPa, then
30 DEG C are cooled to, low whipping speed is to stir 30min under 10r/s, obtains fire prevention glue.
（5）Deionized water is filled into preprepared double layer glass cavity, is placed in 1h in 80 DEG C of drying box, so
Afterwards by glass taking-up ultrasonic cleaning 1h, then with deionized water carry out secondary cleaning；Again by above-mentioned steps（4）In fireproof gum
Liquid is slowly fed into glass cavity, during which gently taps glass with mallet, to ensure that bubble is discharged, by the mouth silicon that is in the milk after filling
Ketone glass cement is closed, and glass is placed in 80 DEG C of air dry oven, places 15h, is cured fire prevention glue, that is, is prepared into anti-spoke
Penetrate grouting-type flame resistant glass.According to GB15763.1-2001《Safety glass flame resistant glass for building》Test the saturating of flame resistant glass
Light rate and UV resistant performance, and the outer air bubble problem of flame resistant glass is observed, it is resistance to then will to characterize its in glass merging Muffle furnace
Fire screen is hot.
The flame resistant glass light transmittance 86.6 of gained, after ultraviolet light irradiates, light transmittance variation is 5.1%, and microvesicle is few, and
And fire resistance period reaches 105min.
Embodiment 5
(1) by 70 parts of Ludox, 14 parts of polyalcohol, 3 parts of surfactant, 3 parts three mouthfuls of burnings of preservative addition
In bottle, temperature is 60 DEG C, heating water bath stirs 1h under rotating speed 20r/s.
（2）It is 1 in mass ratio:1 weighs dimethyl silicone polymer and 2- alkylols, is stirred evenly at normal temperatures with glass bar
Obtain Compounded Antifoamer.
（3）By above-mentioned steps（2）Compounded Antifoamer add in above-mentioned steps（1）Mix silica sol in, temperature be 60
DEG C, rotating speed to stir 20min under 20r/s, be then evacuated to 0.05MPa, and be stirred under vacuum 20min, obtain stable and uniform
Ludox dispersion liquid.
（4）15 parts of KOH are taken, a concentration of 50% solution is made, is slowly added to above-mentioned steps（3）In Ludox point
In dispersion liquid, temperature for 60 DEG C, mixing speed 50min is stirred under 30r/s, 10min is then stirred under 0.05MPa, then
30 DEG C are cooled to, low whipping speed is to stir 30min under 10r/s, obtains fire prevention glue.
（5）Deionized water is filled into preprepared double layer glass cavity, is placed in 1h in 80 DEG C of drying box, so
Afterwards by glass taking-up ultrasonic cleaning 1h, then with deionized water carry out secondary cleaning；Again by above-mentioned steps（4）In fireproof gum
Liquid is slowly fed into glass cavity, during which gently taps glass with mallet, to ensure that bubble is discharged, by the mouth silicon that is in the milk after filling
Ketone glass cement is closed, and glass is placed in 80 DEG C of air dry oven, places 15h, is cured fire prevention glue, that is, is prepared into anti-spoke
Penetrate grouting-type flame resistant glass.According to GB15763.1-2001《Safety glass flame resistant glass for building》Test the saturating of flame resistant glass
Light rate and UV resistant performance, and the outer air bubble problem of flame resistant glass is observed, it is resistance to then will to characterize its in glass merging Muffle furnace
Fire screen is hot.
The flame resistant glass light transmittance 86.2 of gained, after ultraviolet light irradiates, light transmittance variation is 5.1%, and microvesicle is few, and
And fire resistance period reaches 112min.
Embodiment 6
(1) by 70 parts of Ludox, 15 parts of polyalcohol, 3 parts of surfactant, 3 parts three mouthfuls of burnings of preservative addition
In bottle, temperature is 60 DEG C, heating water bath stirs 1h under rotating speed 20r/s.
（2）It is 1 in mass ratio:1 weighs dimethyl silicone polymer and 2- alkylols, is stirred evenly at normal temperatures with glass bar
Obtain Compounded Antifoamer.
（3）By above-mentioned steps（2）Compounded Antifoamer add in above-mentioned steps（1）Mix silica sol in, temperature be 60
DEG C, rotating speed to stir 20min under 20r/s, be then evacuated to 0.05MPa, and be stirred under vacuum 20min, obtain stable and uniform
Ludox dispersion liquid.
（4）15 parts of KOH are taken, a concentration of 50% solution is made, is slowly added to above-mentioned steps（3）In Ludox point
In dispersion liquid, temperature for 60 DEG C, mixing speed 50min is stirred under 30r/s, 10min is then stirred under 0.05MPa, then
30 DEG C are cooled to, low whipping speed is to stir 30min under 10r/s, obtains fire prevention glue.
（5）Deionized water is filled into preprepared double layer glass cavity, is placed in 1h in 80 DEG C of drying box, so
Afterwards by glass taking-up ultrasonic cleaning 1h, then with deionized water carry out secondary cleaning；Again by above-mentioned steps（4）In fireproof gum
Liquid is slowly fed into glass cavity, during which gently taps glass with mallet, to ensure that bubble is discharged, by the mouth silicon that is in the milk after filling
Ketone glass cement is closed, and glass is placed in 80 DEG C of air dry oven, places 15h, is cured fire prevention glue, that is, is prepared into anti-spoke
Penetrate grouting-type flame resistant glass.According to GB15763.1-2001《Safety glass flame resistant glass for building》Test the saturating of flame resistant glass
Light rate and UV resistant performance, and the outer air bubble problem of flame resistant glass is observed, it is resistance to then will to characterize its in glass merging Muffle furnace
Fire screen is hot.
The flame resistant glass light transmittance 86.7 of gained, after ultraviolet light irradiates, light transmittance variation is 5.7%, and microvesicle is few, and
And fire resistance period reaches 109min.
Claims (8)
1. a kind of preparation method of no microvesicle radioresistance grouting-type flame resistant glass, the preparation method is by raw material composition and its matter
Amount part content follows these steps to carry out：
（1）By 70 part 50% of Ludox, 15 parts of polyalcohols, 2 parts of surfactants, 2 parts of preservative added in three-necked flask,
In the case where temperature is 60 DEG C, rotating speed is 20r/s, heating water bath stirs 1h；
（2）By 1:1 weighs dimethyl silicone polymer and 2- alkylols, stirs evenly acquisition compounding defoaming with glass bar at normal temperatures
Agent；
（3）By above-mentioned steps（2）Compounded Antifoamer add in above-mentioned steps（1）Mix silica sol in, temperature be 60 DEG C, turns
Then speed is evacuated to 0.05MPa, and vacuumize stirring 10min, the silicon for obtaining stable and uniform is molten to stir 10min under 15r/s
Glue dispersion liquid；
（4）15 parts of KOH is taken, a concentration of 50% solution is made, is slowly added to above-mentioned steps（3）Ludox dispersion liquid
In, it is 60 DEG C in temperature, mixing speed stirs 50min under 30r/s, and 10min is then stirred under 0.05MPa, is then cooled down
To 30 DEG C, then low whipping speed obtains fire prevention glue to stir 30min under 10r/s；
（5）Deionized water is filled into preprepared double layer glass cavity, is placed in 1h in 80 DEG C of drying box, then will
Glass, which takes out, uses ultrasonic cleaning 1h, then carry out secondary cleaning with deionized water；By above-mentioned steps（4）In fire prevention glue it is slow
It is fed into glass cavity, during which gently taps glass with mallet, so that bubble is discharged, will be in the milk mouth with silicone glass cement after filling
Closing, glass is placed in 80 DEG C of air dry oven, places 12h, and fire prevention glue is allowed to cure, and is obtained no microvesicle radioresistance and is filled
Slurry type flame resistant glass.
2. preparation method as described in claim 1, the Ludox is alkaline silica sol, content 50%, grain size 100nm.
3. preparation method as described in claim 1, the polyalcohol be ethylene glycol, glycerine, two polyethylene glycol, propylene glycol and
One kind or combination thereof in two polypropylene glycols.
4. preparation method as described in claim 1, the surfactant is dimethyl silicone polymer, glycerol monostearate
One kind or combination thereof in ester, fatty acid sorbitan and polysorbate.
5. preparation method as described in claim 1, the preservative is one in tin oxide, phosphorous oxide, zinc oxide and borax
Kind or combination thereof.
6. preparation method as described in claim 1, the 2- alkylols be isopropanol, 2- butanol, one kind in 2- amylalcohols or
Combination thereof.
7. preparation method as described in claim 1, the total addition level of the Compounded Antifoamer is 4 parts, wherein Compounded Antifoamer
It is made of isopropanol and dimethyl silicone polymer, mass ratio is 1:1.
8. a kind of preparation method as described in claim 1, the preparation method are answered by isopropanol and dimethyl silicone polymer
Antifoaming agent is manufactured, is cured with KOH, works as SiO2It is 9 in molar ratio with KOH:When 4, flame resistant glass light transmittance obtained is
86.6%。
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| CN107813549A (en) * | 2017-10-23 | 2018-03-20 | 秦皇岛玻璃工业研究设计院有限公司 | One kind fire prevention anti-electromagnetic radiation glass and preparation method thereof |
| CN109111111A (en) * | 2018-10-18 | 2019-01-01 | 中山市中佳新材料有限公司 | Single-sheet fire-resistant glass and preparation method thereof |
| CN110627383B (en) * | 2019-10-30 | 2022-05-10 | 应急管理部天津消防研究所 | Preparation method of transparent fireproof gel and composite fireproof glass |
| CN113561584B (en) * | 2020-04-29 | 2023-02-28 | 吉林省峰海工贸有限公司 | Ultralow-temperature pouring sealant fireproof glass and preparation method thereof |
| CN112320807B (en) * | 2020-11-26 | 2022-10-14 | 上海新安纳电子科技有限公司 | Modified silica sol, fireproof liquid, composite fireproof glass and preparation method and application thereof |
| CN113429983B (en) * | 2021-06-23 | 2022-05-10 | 应急管理部天津消防研究所 | High-fire-resistance transparent fireproof gel, preparation method thereof and composite fireproof glass |
| CN113844120A (en) * | 2021-09-28 | 2021-12-28 | 广东阿特斯科技有限公司 | Production process of rubbing mobile phone back plate |
| CN114409279B (en) * | 2022-01-24 | 2024-03-29 | 广东卫屋防火科技有限公司 | Fireproof interlayer adhesive, preparation method thereof and fireproof glass comprising fireproof interlayer adhesive |
| CN115370272A (en) * | 2022-09-20 | 2022-11-22 | 江苏铁锚玻璃股份有限公司 | High-light-transmittance heat-insulation fireproof glass and preparation method thereof |
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| CN104645673A (en) * | 2013-11-19 | 2015-05-27 | 青岛欧美亚橡胶工业有限公司 | A preparing method of an organosilicon defoamer specially used for gel laminated fire-resistance glass |
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