CN105835512A - Preparation method of micro-bubble-free anti-radiation grouted fireproof glass - Google Patents
Preparation method of micro-bubble-free anti-radiation grouted fireproof glass Download PDFInfo
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- CN105835512A CN105835512A CN201610176134.8A CN201610176134A CN105835512A CN 105835512 A CN105835512 A CN 105835512A CN 201610176134 A CN201610176134 A CN 201610176134A CN 105835512 A CN105835512 A CN 105835512A
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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
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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
- 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
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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
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Joining Of Glass To Other Materials (AREA)
- Fireproofing Substances (AREA)
- Floor Finish (AREA)
Abstract
A preparation method of micro-bubble-free anti-radiation grouted fireproof glass includes the following steps: adding polyols, a surfactant and a preservative to silicon sol with uniform stirring; uniformly mixing polydimethylsiloxane and 2-alkyl alcohol to prepare a compound defoamer and adding the compound defoamer to the silicon sol mixture, and vacuumizing and stirring the mixed liquid to prepare stable and uniform silicon sol dispersion liquid; adding a KOH dilution liquid to the silicon sol dispersion liquid with uniform stirring; and grouting sandwich glass with the liquid mixture and performing high-temperature curing to prepare the grouted fireproof glass. With the compound of the isopropyl alcohol and the polydimethylsiloxane as a defoamer for curing the glass, the transmittance of the fireproof glass reaches 86.6% and is changed into 5.8% when the glass is irradiated by UV light. The glass has very few bubbles. The method effectively improves the problem of poor weather resistance and too many bubbles in the grouted fireproof glass with polyacrylamide as a sandwich glue in the prior art.
Description
Technical field
The present invention relates to the preparation method of a kind of flame resistant glass, especially a kind of without microvesicle radioprotective grouting-type flame resistant glass
Preparation method.
Background technology
Grouting-type flame resistant glass is generally by the above original sheet glass of two-layer, and surrounding seals with flame-retardant rubber strip, middle perfusion fire prevention
Glue is constituted.Traditional fire prevention glue mainly based on acrylamides, add initiator, coupling agent and other help
Agent.Owing to use and the acrylamide self of coupling agent are organic reasons, can to glass product bring bubble, fission,
Turn white, UV resistant performance difference defect, have a strong impact on its serviceability.
CN104513032A discloses " a kind of flame resistant glass clear gel formula ".Its each component accounts for gross mass percentage
Number is respectively as follows: ethanolamine 4-25%, initiator 0.1-3%, magnesium chloride 5-20%, gel 5-20%, ammonium phosphate 5-20%, carbamide 2-
30%, boric acid 1-15%, sodium chloride 2-20%, surplus is water.Gellant mainly has acrylamide and vinyl alcohol, this Organic substance conduct
Primary raw material causes flame resistant glass UV resistant performance to weaken, the most aging；The inorganic salts such as ammonium phosphate, boric acid, sodium chloride big
Amount addition have impact on the light transmittance of flame resistant glass and can produce bubble in whipping process, does not contains froth breaking in this formula simultaneously
Agent also results in the generation of bubble in whipping process, and the use of initiator also can make gellant produce bubble in cross-linking process.
CN102515574A discloses " preparation method of a kind of gel interlayer fireproofing glass ".The transparent fireproof of this flame resistant glass coagulates
Glue mainly includes machine gellant acrylamide, cross-linking agent, initiator, ammonium phosphate, magnesium chloride, sucrose, urea element, ethanolamine and steaming
Distilled water.Acrylamide is primary raw material, but the UV resistant performance of flame resistant glass can be made to weaken as Organic substance；Cross-linking agent and
Initiator can produce a large amount of bubble in organic polymer whipping process；Ammonium phosphate, magnesium chloride, sucrose, urea are plain and ethanolamine
A large amount of uses have had a strong impact on the light transmittance of glass.
KR2011136705A discloses " resin Composition of a kind 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 this component does not has the use of defoamer, the most inevitably brings a large amount of bubble to flame resistant glass；This patent does not has
Light transmittance, UV resistant irradiation performance are detected.
Summary of the invention
The concrete technical problems that the invention solves the problems that is the frit selecting stable performance, prepares suitable compounding froth breaking
Agent and resistant to elevated temperatures fire prevention slurry, and the preparation method of a kind of grouting-type flame resistant glass of radioprotective without microvesicle is provided.
In order to achieve the above object, the technical solution adopted in the present invention is as follows:
The preparation method of a kind of grouting-type flame resistant glass of radioprotective without microvesicle, presses following step by raw material composition and mass parts content thereof
Suddenly carry out:
(1) by the Ludox of 60 ~ 80 parts, the polyhydric alcohol of 10 ~ 15 parts, the surfactant of 1 ~ 3 part, the preservative of 1-2 part adds
In there-necked flask, temperature be 60 DEG C, heating in water bath stirring 1h under rotating speed 20r/s.
(2) weigh polydimethylsiloxane and 2-alkylol for 1:1 in mass ratio, stir with Glass rod at normal temperatures
Obtain Compounded Antifoamer.
(3) Compounded Antifoamer of above-mentioned steps (2) is added in the mix silica sol of above-mentioned steps (1), be 60 in temperature
DEG C, rotating speed be under 15r/s stirring 10min, be then evacuated to 0.05MPa, and vacuum stirring 10min, it is thus achieved that stable and uniform
Ludox dispersion liquid.
(4) take 10-17 part KOH, make the solution that concentration is 50%, be slowly added to the Ludox in above-mentioned steps (3)
In dispersion liquid, temperature be 60 DEG C, mixing speed at 30r/s under stir 50min, under 0.05MPa, then stir 10min, connect
And be cooled to 30 DEG C, low whipping speed is stirring 30min under 10r/s, i.e. prepares fire prevention glue.
(5) deionized water is filled preprepared double layer glass cavity, be placed in 1h in the drying baker of 80 DEG C, so
After by glass taking-up ultrasonic waves for cleaning 1h, then carry out secondary cleaning with deionized water；Again by the Waterproof gum in above-mentioned steps (4)
Liquid is slowly fed into glass intracavity, and period taps glass gently with mallet, to ensure that bubble is discharged, by grouting mouth silicon after filling
Ketone glass cement is closed, and is placed in by glass in the air dry oven of 80 DEG C, places 12h, makes Waterproof gum liquid-solidization, be i.e. prepared into anti-spoke
Penetrate grouting-type flame resistant glass.
Further, described preparation method is to follow these steps to carry out by raw material composition and mass parts content thereof:
(1) by the Ludox of 80 part 50%, 15 parts of polyhydric alcohol, 2 parts of surfactants, the preservative of 2 parts adds in there-necked flask,
Temperature be 60 DEG C, rotating speed be heating in water bath stirring 1h under 20r/s.
(2) weighing polydimethylsiloxane and 2-alkylol by 1:1, stirring with Glass rod at normal temperatures, it is compounding to obtain
Defoamer.
(3) Compounded Antifoamer of above-mentioned steps (2) is added in the mix silica sol of above-mentioned steps (1), be 60 in temperature
DEG C, rotating speed be stirring 10min under 15r/s, be then evacuated to 0.05MPa, and evacuation stirring 10min, it is thus achieved that stable and uniform
Ludox dispersion liquid.
(4) take the KOH of 15.5 parts, make the solution that concentration is 50%, be slowly added to the Ludox of above-mentioned steps (3)
In dispersion liquid, being 60 DEG C in temperature, mixing speed stirs 50min under 30r/s, then stirs 10min under 0.05MPa, so
After be cooled to 30 DEG C, then low whipping speed be under 10r/s stirring 30min, i.e. obtain fire prevention glue.
(5) deionized water is filled preprepared double layer glass cavity, be placed in 1h in the drying baker of 80 DEG C, so
After by glass taking-up ultrasonic waves for cleaning 1h, then carry out secondary cleaning with deionized water；By the fire prevention glue in above-mentioned steps (4)
Slowly being fed into glass intracavity, period taps glass gently with mallet, so that bubble is discharged, will fill with silicone glass cement after filling
Slurry mouth is closed, and is placed in by glass in the air dry oven of 80 DEG C, places 12h, allows Waterproof gum liquid-solidization, i.e. prepares without the anti-spoke of microvesicle
Penetrate grouting-type flame resistant glass.
Additional technical feature in technique scheme is as follows.
Described Ludox is alkaline silica sol, and content is 50%, and particle diameter is 100nm.
Described polyhydric alcohol be the one in ethylene glycol, glycerol, two Polyethylene Glycol, propylene glycol and two polypropylene glycols or it
Combination.
Described surfactant is that polydimethylsiloxane, glyceryl monostearate, fatty acid Pyrusussuriensis be smooth and Polysorbate
In one or combinations thereof.
Described preservative is to be the one in stannum oxide, phosphorous oxide, zinc oxide and Borax or combinations thereof.
Described 2-alkylol is the one in isopropanol, 2-butanol, 2-amylalcohol or combinations thereof.
The total addition level of described Compounded Antifoamer is 4 parts, and wherein Compounded Antifoamer is by isopropanol and polydimethylsiloxanes
Alkane forms, and its mass ratio is 1:1.
Described preparation method is to be done defoamer by isopropanol and polydimethylsiloxane are compounding, solidifies with KOH, when
SiO2With during the ratio of KOH during 9:4, prepared flame resistant glass light transmittance is 86.6%.
Implement the preparation method of a kind of grouting-type flame resistant glass of radioprotective without microvesicle that the invention described above is provided, use silicon
Colloidal sol and KOH raw material, further increase ultra-violet radiation resisting and high temperature resistant；Isopropanol and polydimethylsiloxane is used to compound
As defoamer, it is suppressed that the generation of bubble, and solidify with KOH, it is achieved that a kind of light transmittance is high, ultra-violet radiation resisting
By force, resistant to elevated temperatures method for glass preparation.
In such scheme of the present invention, work as SiO2When being 9:4 with the ratio of KOH, specifying according to GB15763.1, utilization can
See light thoroughly/reflectance test instrument, resistance to irradiation box and repacking Muffle furnace light transmittance, UV resistant performance and Nai Gao to flame resistant glass
Warm nature can be detected, and is up to 86.6% through recording flame resistant glass light transmittance, and after ultraviolet irradiates, light transmittance is changed to 5.8%,
Fire resistance period reaches 90min, effectively improves the resistance to of traditional grouting-type flame resistant glass with polyacrylamide as squeegee
The phenomenon that time property difference is many with bubble.
Accompanying drawing explanation
Fig. 1 is the schematic perspective view of the grouting-type flame resistant glass of radioprotective without microvesicle that this method prepares.In figure: 1 and 2 is two
The sheet glass on limit；3 is flame retardant sealant bar.
Fig. 2 is the flame resistant glass pictorial diagram not adding defoamer.
Fig. 3 is the flame resistant glass pictorial diagram adding defoamer.
Detailed description of the invention
Below the detailed description of the invention of the present invention is further illustrated.
Implement the preparation method of a kind of grouting-type flame resistant glass of radioprotective without microvesicle, the constituent of the method fire prevention glue
Including alkaline silica sol, Compounded Antifoamer, polyhydric alcohol, surfactant, preservative, deionized water.Wherein alkaline silica sol
SiO2Content is 50%, and particle diameter is 100nm；Described polyhydric alcohol is ethylene glycol, glycerol, two Polyethylene Glycol, propylene glycol and dimerization third
One in glycol or combinations thereof；Described surfactant is polydimethylsiloxane, glyceryl monostearate, fatty acid
Pyrusussuriensis is smooth and the one in Polysorbate or combinations thereof；Described preservative is in stannum oxide, phosphorous oxide, zinc oxide and Borax
One or combinations thereof；Described 2-alkylol is the one in isopropanol, 2-butanol, 2-amylalcohol or combinations thereof；
Described Compounded Antifoamer is prepared for 1:1 with polydimethylsiloxane in mass ratio by isopropanol.Slurry agitation is uniform, and add
Enter the KOH solution that concentration is 50%, work as SiO2When being 9:4 with the molar ratio of KOH, prepared flame resistant glass light transmittance reaches
86.6%, after ultraviolet irradiates 100 hours, light transmittance is changed to 5.8%, and flame resistant glass bubble is few, effectively improves traditional
The situation that grouting-type flame resistant glass weatherability is poor, bubble is many with polyacrylamide as squeegee.Detailed description of the invention is as follows.
(1) by the Ludox of 60 ~ 80 parts, the polyhydric alcohol of 10 ~ 15 parts, the surfactant of 1 ~ 3 part, the preservative of 1-2 part
Add in there-necked flask, temperature be 60 DEG C, heating in water bath stirring 1h under rotating speed 20r/s；
(2) weigh polydimethylsiloxane and 2-alkylol for 1:1 in mass ratio, stir acquisition with Glass rod at normal temperatures
Compounded Antifoamer.
(3) Compounded Antifoamer 3 ~ 6 parts of above-mentioned steps (2) is added in the mix silica sol of above-mentioned steps (1), in temperature
Be 60 DEG C, rotating speed be stirring 10min under 15r/s, be then evacuated to 0.05MPa, and vacuum stirring 10min, it is thus achieved that stable all
Even Ludox dispersion liquid.
(4) take 10 ~ 17 parts of KOH, make the solution that concentration is 50%, be slowly added to the Ludox in above-mentioned steps (3)
In dispersion liquid, temperature be 60 DEG C, mixing speed at 30r/s under stir 50min, under 0.05MPa, then stir 10min, connect
And be cooled to 30 DEG C, low whipping speed is stirring 30min under 10r/s, i.e. prepares fire prevention glue.
(5) deionized water is filled preprepared double layer glass cavity, be placed in 1h in the drying baker of 80 DEG C, so
After by glass taking-up ultrasonic waves for cleaning 1h, then carry out secondary cleaning with deionized water；Again by the Waterproof gum in above-mentioned steps (4)
Liquid is slowly fed into glass intracavity, and period taps glass gently with mallet, to ensure that bubble is discharged, by grouting mouth silicon after filling
Ketone glass cement is closed, and is placed in by glass in the air dry oven of 80 DEG C, places 12h, makes Waterproof gum liquid-solidization, be i.e. prepared into anti-spoke
Penetrate grouting-type flame resistant glass.Printing opacity according to GB15763.1-2001 " safety glass flame resistant glass for building " test flame resistant glass
Rate and UV resistant performance, and observe the outer air bubble problem of flame resistant glass, then insert glass that to characterize it in Muffle furnace fire-resistant
Thermal insulation.
The detailed description of the invention of the present invention is further illustrated by following example, and the invention is not restricted to these and implement
Example.
Embodiment 1
(1) by the Ludox of 70 parts, the polyhydric alcohol of 10 parts, the surfactant of 1 part, the preservative of 1 part adds there-necked flask
In, temperature be 60 DEG C, heating in water bath stirring 1h under rotating speed 20r/s.
(2) weigh polydimethylsiloxane and 2-alkylol for 1:1 in mass ratio, stir with Glass rod at normal temperatures
Obtain Compounded Antifoamer.
(3) Compounded Antifoamer of above-mentioned steps (2) is added in the mix silica sol of above-mentioned steps (1), be 60 in temperature
DEG C, rotating speed be under 15r/s stirring 10min, be then evacuated to 0.05MPa, and vacuum stirring 10min, it is thus achieved that stable and uniform
Ludox dispersion liquid.
(4) taking 15 parts of KOH, make the solution that concentration is 50%, the Ludox being slowly added in above-mentioned steps (3) divides
Dissipate in liquid, temperature be 60 DEG C, mixing speed at 30r/s under stir 50min, under 0.05MPa, then stir 10min, then
Being cooled to 30 DEG C, low whipping speed is stirring 30min under 10r/s, i.e. prepares fire prevention glue.
(5) deionized water is filled preprepared double layer glass cavity, be placed in 1h in the drying baker of 80 DEG C, so
After by glass taking-up ultrasonic waves for cleaning 1h, then carry out secondary cleaning with deionized water；Again by the Waterproof gum in above-mentioned steps (4)
Liquid is slowly fed into glass intracavity, and period taps glass gently with mallet, to ensure that bubble is discharged, by grouting mouth silicon after filling
Ketone glass cement is closed, and is placed in by glass in the air dry oven of 80 DEG C, places 12h, makes Waterproof gum liquid-solidization, be i.e. prepared into anti-spoke
Penetrate grouting-type flame resistant glass.The saturating of flame resistant glass is tested according to GB15763.1-2001 " safety glass flame resistant glass for building "
Light rate and UV resistant performance, and observe the outer air bubble problem of flame resistant glass, then insert glass that to characterize it in Muffle furnace resistance to
Fire screen is hot.
The flame resistant glass light transmittance 86.5 of gained, after ultraviolet irradiates, light transmittance is changed to 5.5%, and microvesicle is few, and
And fire resistance period reaches 100min.
Embodiment 2
(1) by the Ludox of 70 parts, the polyhydric alcohol of 11 parts, the surfactant of 2 parts, the preservative of 2 parts adds there-necked flask
In, temperature be 60 DEG C, heating in water bath stirring 1h under rotating speed 20r/s.
(2) weigh polydimethylsiloxane and 2-alkylol for 1:1 in mass ratio, stir with Glass rod at normal temperatures
Obtain Compounded Antifoamer.
(3) Compounded Antifoamer of above-mentioned steps (2) is added in the mix silica sol of above-mentioned steps (1), be 60 in temperature
DEG C, rotating speed be under 15r/s stirring 15min, be then evacuated to 0.05MPa, and vacuum stirring 15min, it is thus achieved that stable and uniform
Ludox dispersion liquid.
(4) taking 15 parts of KOH, make the solution that concentration is 50%, the Ludox being slowly added in above-mentioned steps (3) divides
Dissipate in liquid, temperature be 60 DEG C, mixing speed at 30r/s under stir 50min, under 0.05MPa, then stir 10min, then
Being cooled to 30 DEG C, low whipping speed is stirring 30min under 10r/s, i.e. prepares fire prevention glue.
(5) deionized water is filled preprepared double layer glass cavity, be placed in 1h in the drying baker of 80 DEG C, so
After by glass taking-up ultrasonic waves for cleaning 1h, then carry out secondary cleaning with deionized water；Again by the Waterproof gum in above-mentioned steps (4)
Liquid is slowly fed into glass intracavity, and period taps glass gently with mallet, to ensure that bubble is discharged, by grouting mouth silicon after filling
Ketone glass cement is closed, and is placed in by glass in the air dry oven of 80 DEG C, places 12h, makes Waterproof gum liquid-solidization, be i.e. prepared into anti-spoke
Penetrate grouting-type flame resistant glass.The saturating of flame resistant glass is tested according to GB15763.1-2001 " safety glass flame resistant glass for building "
Light rate and UV resistant performance, and observe the outer air bubble problem of flame resistant glass, then insert glass that to characterize it in Muffle furnace resistance to
Fire screen is hot.
The flame resistant glass light transmittance 86.7 of gained, after ultraviolet irradiates, light transmittance is changed to 5.8%, and microvesicle is few, and
And fire resistance period reaches 110min.
Embodiment 3
(1) by the Ludox of 70 parts, the polyhydric alcohol of 12 parts, the surfactant of 3 parts, the preservative of 3 parts adds there-necked flask
In, temperature be 60 DEG C, heating in water bath stirring 1h under rotating speed 20r/s.
(2) weigh polydimethylsiloxane and 2-alkylol for 1:1 in mass ratio, stir with Glass rod at normal temperatures
Obtain Compounded Antifoamer.
(3) Compounded Antifoamer of above-mentioned steps (2) is added in the mix silica sol of above-mentioned steps (1), be 60 in temperature
DEG C, rotating speed be under 20r/s stirring 15min, be then evacuated to 0.05MPa, and vacuum stirring 15min, it is thus achieved that stable and uniform
Ludox dispersion liquid.
(4) taking 15 parts of KOH, make the solution that concentration is 50%, the Ludox being slowly added in above-mentioned steps (3) divides
Dissipate in liquid, temperature be 60 DEG C, mixing speed at 30r/s under stir 50min, under 0.05MPa, then stir 10min, then
Being cooled to 30 DEG C, low whipping speed is stirring 30min under 10r/s, i.e. prepares fire prevention glue.
(5) deionized water is filled preprepared double layer glass cavity, be placed in 1h in the drying baker of 80 DEG C, so
After by glass taking-up ultrasonic waves for cleaning 1h, then carry out secondary cleaning with deionized water；Again by the Waterproof gum in above-mentioned steps (4)
Liquid is slowly fed into glass intracavity, and period taps glass gently with mallet, to ensure that bubble is discharged, by grouting mouth silicon after filling
Ketone glass cement is closed, and is placed in by glass in the air dry oven of 80 DEG C, places 15h, makes Waterproof gum liquid-solidization, be i.e. prepared into anti-spoke
Penetrate grouting-type flame resistant glass.The saturating of flame resistant glass is tested according to GB15763.1-2001 " safety glass flame resistant glass for building "
Light rate and UV resistant performance, and observe the outer air bubble problem of flame resistant glass, then insert glass that to characterize it in Muffle furnace resistance to
Fire screen is hot.
The flame resistant glass light transmittance 86.3 of gained, after ultraviolet irradiates, light transmittance is changed to 5.4%, and microvesicle is few, and
And fire resistance period reaches 107min.
Embodiment 4
(1) by the Ludox of 70 parts, the polyhydric alcohol of 13 parts, the surfactant of 3 parts, the preservative of 3 parts adds there-necked flask
In, temperature be 60 DEG C, heating in water bath stirring 1h under rotating speed 20r/s.
(2) weigh polydimethylsiloxane and 2-alkylol for 1:1 in mass ratio, stir with Glass rod at normal temperatures
Obtain Compounded Antifoamer.
(3) Compounded Antifoamer of above-mentioned steps (2) is added in the mix silica sol of above-mentioned steps (1), be 60 in temperature
DEG C, rotating speed be under 20r/s stirring 15min, be then evacuated to 0.05MPa, and vacuum stirring 15min, it is thus achieved that stable and uniform
Ludox dispersion liquid.
(4) taking 15 parts of KOH, make the solution that concentration is 50%, the Ludox being slowly added in above-mentioned steps (3) divides
Dissipate in liquid, temperature be 60 DEG C, mixing speed at 30r/s under stir 50min, under 0.05MPa, then stir 10min, then
Being cooled to 30 DEG C, low whipping speed is stirring 30min under 10r/s, i.e. prepares fire prevention glue.
(5) deionized water is filled preprepared double layer glass cavity, be placed in 1h in the drying baker of 80 DEG C, so
After by glass taking-up ultrasonic waves for cleaning 1h, then carry out secondary cleaning with deionized water；Again by the Waterproof gum in above-mentioned steps (4)
Liquid is slowly fed into glass intracavity, and period taps glass gently with mallet, to ensure that bubble is discharged, by grouting mouth silicon after filling
Ketone glass cement is closed, and is placed in by glass in the air dry oven of 80 DEG C, places 15h, makes Waterproof gum liquid-solidization, be i.e. prepared into anti-spoke
Penetrate grouting-type flame resistant glass.The saturating of flame resistant glass is tested according to GB15763.1-2001 " safety glass flame resistant glass for building "
Light rate and UV resistant performance, and observe the outer air bubble problem of flame resistant glass, then insert glass that to characterize it in Muffle furnace resistance to
Fire screen is hot.
The flame resistant glass light transmittance 86.6 of gained, after ultraviolet irradiates, light transmittance is changed to 5.1%, and microvesicle is few, and
And fire resistance period reaches 105min.
Embodiment 5
(1) by the Ludox of 70 parts, the polyhydric alcohol of 14 parts, the surfactant of 3 parts, the preservative of 3 parts adds there-necked flask
In, temperature be 60 DEG C, heating in water bath stirring 1h under rotating speed 20r/s.
(2) weigh polydimethylsiloxane and 2-alkylol for 1:1 in mass ratio, stir with Glass rod at normal temperatures
Obtain Compounded Antifoamer.
(3) Compounded Antifoamer of above-mentioned steps (2) is added in the mix silica sol of above-mentioned steps (1), be 60 in temperature
DEG C, rotating speed be under 20r/s stirring 20min, be then evacuated to 0.05MPa, and vacuum stirring 20min, it is thus achieved that stable and uniform
Ludox dispersion liquid.
(4) taking 15 parts of KOH, make the solution that concentration is 50%, the Ludox being slowly added in above-mentioned steps (3) divides
Dissipate in liquid, temperature be 60 DEG C, mixing speed at 30r/s under stir 50min, under 0.05MPa, then stir 10min, then
Being cooled to 30 DEG C, low whipping speed is stirring 30min under 10r/s, i.e. prepares fire prevention glue.
(5) deionized water is filled preprepared double layer glass cavity, be placed in 1h in the drying baker of 80 DEG C, so
After by glass taking-up ultrasonic waves for cleaning 1h, then carry out secondary cleaning with deionized water；Again by the Waterproof gum in above-mentioned steps (4)
Liquid is slowly fed into glass intracavity, and period taps glass gently with mallet, to ensure that bubble is discharged, by grouting mouth silicon after filling
Ketone glass cement is closed, and is placed in by glass in the air dry oven of 80 DEG C, places 15h, makes Waterproof gum liquid-solidization, be i.e. prepared into anti-spoke
Penetrate grouting-type flame resistant glass.The saturating of flame resistant glass is tested according to GB15763.1-2001 " safety glass flame resistant glass for building "
Light rate and UV resistant performance, and observe the outer air bubble problem of flame resistant glass, then insert glass that to characterize it in Muffle furnace resistance to
Fire screen is hot.
The flame resistant glass light transmittance 86.2 of gained, after ultraviolet irradiates, light transmittance is changed to 5.1%, and microvesicle is few, and
And fire resistance period reaches 112min.
Embodiment 6
(1) by the Ludox of 70 parts, the polyhydric alcohol of 15 parts, the surfactant of 3 parts, the preservative of 3 parts adds there-necked flask
In, temperature be 60 DEG C, heating in water bath stirring 1h under rotating speed 20r/s.
(2) weigh polydimethylsiloxane and 2-alkylol for 1:1 in mass ratio, stir with Glass rod at normal temperatures
Obtain Compounded Antifoamer.
(3) Compounded Antifoamer of above-mentioned steps (2) is added in the mix silica sol of above-mentioned steps (1), be 60 in temperature
DEG C, rotating speed be under 20r/s stirring 20min, be then evacuated to 0.05MPa, and vacuum stirring 20min, it is thus achieved that stable and uniform
Ludox dispersion liquid.
(4) taking 15 parts of KOH, make the solution that concentration is 50%, the Ludox being slowly added in above-mentioned steps (3) divides
Dissipate in liquid, temperature be 60 DEG C, mixing speed at 30r/s under stir 50min, under 0.05MPa, then stir 10min, then
Being cooled to 30 DEG C, low whipping speed is stirring 30min under 10r/s, i.e. prepares fire prevention glue.
(5) deionized water is filled preprepared double layer glass cavity, be placed in 1h in the drying baker of 80 DEG C, so
After by glass taking-up ultrasonic waves for cleaning 1h, then carry out secondary cleaning with deionized water；Again by the Waterproof gum in above-mentioned steps (4)
Liquid is slowly fed into glass intracavity, and period taps glass gently with mallet, to ensure that bubble is discharged, by grouting mouth silicon after filling
Ketone glass cement is closed, and is placed in by glass in the air dry oven of 80 DEG C, places 15h, makes Waterproof gum liquid-solidization, be i.e. prepared into anti-spoke
Penetrate grouting-type flame resistant glass.The saturating of flame resistant glass is tested according to GB15763.1-2001 " safety glass flame resistant glass for building "
Light rate and UV resistant performance, and observe the outer air bubble problem of flame resistant glass, then insert glass that to characterize it in Muffle furnace resistance to
Fire screen is hot.
The flame resistant glass light transmittance 86.7 of gained, after ultraviolet irradiates, light transmittance is changed to 5.7%, and microvesicle is few, and
And fire resistance period reaches 109min.
Claims (9)
1., without a preparation method for microvesicle radioprotective grouting-type flame resistant glass, described preparation method is by raw material composition and matter thereof
Amount part content follows these steps to carry out:
(1) by the Ludox of 60 ~ 80 parts, the polyhydric alcohol of 10 ~ 15 parts, the surfactant of 1 ~ 3 part, the preservative of 1-2 part adds
In there-necked flask, temperature be 60 DEG C, heating in water bath stirring 1h under rotating speed 20r/s；
(2) weigh polydimethylsiloxane and 2-alkylol for 1:1 in mass ratio, stir acquisition with Glass rod at normal temperatures
Compounded Antifoamer；
(3) Compounded Antifoamer of above-mentioned steps (2) is added in the mix silica sol of above-mentioned steps (1), be 60 DEG C, turns in temperature
Speed is stirring 10min under 15r/s, is then evacuated to 0.05MPa, and vacuum stirring 10min, it is thus achieved that the Ludox of stable and uniform
Dispersion liquid；
(4) take 10-17 part KOH, make the solution that concentration is 50%, the Ludox dispersion being slowly added in above-mentioned steps (3)
In liquid, temperature be 60 DEG C, mixing speed at 30r/s under stir 50min, under 0.05MPa, then stir 10min, then drop
Temperature is to 30 DEG C, and low whipping speed is stirring 30min under 10r/s, i.e. prepares fire prevention glue；
(5) deionized water is filled preprepared double layer glass cavity, be placed in 1h in the drying baker of 80 DEG C, then will
Glass takes out and uses ultrasonic waves for cleaning 1h, then carries out secondary cleaning with deionized water；Again the fire prevention glue in above-mentioned steps (4) is delayed
Flood irrigation implantation glass intracavity, period taps glass gently with mallet, to ensure that bubble is discharged, will grouting mouth silicone glass after filling
Glass glue is closed, and is placed in by glass in the air dry oven of 80 DEG C, places 12h, makes Waterproof gum liquid-solidization, i.e. prepares radioprotective grouting
Type flame resistant glass.
2. preparation method as claimed in claim 1, described preparation method is by following by raw material composition and mass parts content thereof
Step is carried out:
(1) by the Ludox of 80 part 50%, 15 parts of polyhydric alcohol, 2 parts of surfactants, the preservative of 2 parts adds in there-necked flask,
Temperature be 60 DEG C, rotating speed be heating in water bath stirring 1h under 20r/s；
(2) weigh polydimethylsiloxane and 2-alkylol by 1:1, stir with Glass rod at normal temperatures and obtain compounding froth breaking
Agent；
(3) Compounded Antifoamer of above-mentioned steps (2) is added in the mix silica sol of above-mentioned steps (1), be 60 DEG C, turns in temperature
Speed is stirring 10min under 15r/s, is then evacuated to 0.05MPa, and evacuation stirring 10min, it is thus achieved that the silicon of stable and uniform
Sol dispersion；
(4) take the KOH of 15.5 parts, make the solution that concentration is 50%, be slowly added to the Ludox dispersion of above-mentioned steps (3)
In liquid, being 60 DEG C in temperature, mixing speed stirs 50min under 30r/s, then stirs 10min under 0.05MPa, then drops
Temperature is to 30 DEG C, then low whipping speed is stirring 30min under 10r/s, i.e. obtains fire prevention glue；
(5) deionized water is filled preprepared double layer glass cavity, be placed in 1h in the drying baker of 80 DEG C, then will
Glass takes out and uses ultrasonic waves for cleaning 1h, then carries out secondary cleaning with deionized water；By slow for the fire prevention glue in above-mentioned steps (4)
Being fed into glass intracavity, period taps glass gently with mallet, so that bubble is discharged, will be in the milk mouth with silicone glass cement after filling
Close, glass is placed in the air dry oven of 80 DEG C, place 12h, allow Waterproof gum liquid-solidization, i.e. prepare without the filling of microvesicle radioprotective
Slurry type flame resistant glass.
3. preparation method as claimed in claim 1 or 2, described Ludox is alkaline silica sol, and content is 50%, and particle diameter is
100nm。
4. preparation method as claimed in claim 1 or 2, described polyhydric alcohol be ethylene glycol, glycerol, two Polyethylene Glycol, the third two
One in alcohol and two polypropylene glycols or combinations thereof.
5. preparation method as claimed in claim 1 or 2, described surfactant is that polydimethylsiloxane, monostearate are sweet
Grease, fatty acid Pyrusussuriensis be smooth and the one in Polysorbate or combinations thereof.
6. preparation method as claimed in claim 1 or 2, described preservative is in stannum oxide, phosphorous oxide, zinc oxide and Borax
One or combinations thereof.
7. preparation method as claimed in claim 1 or 2, described 2-alkylol is the one in isopropanol, 2-butanol, 2-amylalcohol
Or combinations thereof.
8. preparation method as claimed in claim 1 or 2, the total addition level of described Compounded Antifoamer is 4 parts, wherein compounds froth breaking
Agent is made up of with polydimethylsiloxane isopropanol, and its mass ratio is 1:1.
9. preparation method as claimed in claim 1 or 2, described preparation method is to be compounded by isopropanol and polydimethylsiloxane
Do defoamer, solidify with KOH, work as SiO2With during the ratio of KOH during 9:4, prepared flame resistant glass light transmittance is 86.6%.
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| 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 |
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| 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 |
| CN110627383A (en) * | 2019-10-30 | 2019-12-31 | 应急管理部天津消防研究所 | Preparation method of transparent fireproof gel and composite fireproof glass |
| CN113561584A (en) * | 2020-04-29 | 2021-10-29 | 吉林省峰海工贸有限公司 | Ultralow-temperature pouring sealant fireproof glass and preparation method thereof |
| 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 |
| CN112320807A (en) * | 2020-11-26 | 2021-02-05 | 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 |
| CN113429983A (en) * | 2021-06-23 | 2021-09-24 | 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 |
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