Fire-resistant fluid of composite fireproof glass and preparation method thereof and composite fireproof glass
Technical field
The present invention relates to safety glass field more particularly to a kind of fire-resistant fluid of composite fireproof glass and preparation method thereof and
The composite fireproof glass prepared using the fire-resistant fluid.
Background technique
Safety glass is a kind of important New Building Materials, be broadly divided into toughened glass, laminated glass, bulletproof glass,
Burglar-proof glazing, flame resistant glass, wire glass, protective glass and pad pasting glass;Flame resistant glass is a kind of building with fire-proof function
Exterior wall or door glass are built, it is able to maintain the long period under 1000 DEG C of flame impingements and does not burst, to effectively prevent flame
With the sprawling of smog, be conducive to find fire behavior at the first time, guarantee that disaster-stricken crowd has the sufficiently long time to withdraw scene, and to rescue
The time has been striven in calamity work, is current most effective safest fire prevention class glass product;Flame resistant glass is divided into composite fireproof glass
And single-sheet fire-resistant glass, composite fireproof glass refer to ordinary plate glass more than two panels or two panels transparent fireproof adhesive
Glass made of bonding or the glass for spraying composite fireproof glass liquid, composite fireproof glass have fire integrity and resistance to fire screen
It is hot, also there are the superperformances such as high mechanical strength, anti-folding, resistance to compression, its glue-line meeting of preventing fires when composite fireproof glass encounters fire
Rapid foaming and intumescing forms the refractory heat-insulating froth bed of hard insulation, and a large amount of heats for absorbing fire and generating effectively block flame,
Completely cut off high temperature and pernicious gas, while glue-line of preventing fires can also bond broken sheet glass, to keep whole integrality;Fire prevention
The performance of glue-line decides the performance of composite fireproof glass, and glue-line of preventing fires be solidified by fire-resistant fluid, therefore fire-resistant fluid whether
Decide whether composite fireproof glass has preferable fire protecting performance with preferable performance.
The work that the fire-resistant fluid of composite fireproof glass does in the country at present is in phase of basic research, and the country is widely used
Be inorganic fire liquid, such as sodium silicate aqueous solution or potassium silicate aqueous solution, be commonly called as sodium silicate or potassium water glass, and for inorganic
It is less with the fire-resistant fluid research of organic composite material preparation.
There are many shortcomings in fireproof gum made of being solidified in the prior art as fire-resistant fluid, such as in terms of fire protecting performance
Waterglass, modulus is low, and solid content is low, and water content is big, and then results in composite fireproof glass that there is a large amount of microvesicles, directly
Affect apparent mass, optical property, hardness and the toughness of composite fireproof glass, it is often more important that the presence of microvesicle substantially reduces
The fire protecting performance of composite fireproof glass, has seriously affected the using effect and service life of composite fireproof glass.
Summary of the invention
In view of this, the embodiment of the invention provides a kind of preparation method of the fire-resistant fluid of composite fireproof glass, main mesh
Be to provide made of a kind of fire-resistant fluid as the composite fireproof glass solidifies without microvesicle and the good fireproof gum of fire protecting performance.
In order to achieve the above objectives, invention broadly provides following technical solutions:
On the one hand, the present invention provides a kind of preparation methods of the fire-resistant fluid of composite fireproof glass, comprising the following steps:
(1) by weight, by 15-35 parts of polyalcohols, 15-50 parts of function monomers, 2-14 parts of heat-resisting stabilizing agents, 0.05-
0.3 part of curing agent, 2-8 parts of carbon forming agents and 8-20 parts of deionized waters are mixed, agitated that the first mixed emulsion is made;
By weight, by 30-40 parts of first mixed emulsions and 20-40 parts of hydrophilic nano silica dioxide granules into
Row mixing, agitated obtained nanometer silicon dioxide particle dispersion emulsion;
(2) by weight, by 10-30 parts of styrene, 15-40 parts of methyl methacrylates and 20-50 parts of acrylic acid fourths
Ester is mixed, agitated that the second mix monomer lotion is made;
By weight, by 1-8 parts of the second mix monomer lotions, 0.01-0.025 parts of emulsifiers, 0.1-0.7 parts of friendships
Connection agent and 5-15 parts of deionized waters be added in the 50-80 parts of nanometer silicon dioxide particle dispersion emulsions, and be heated to 60 DEG C-
65 DEG C, then 0.01-0.05 parts of redox type initiators are added into the nanometer silicon dioxide particle dispersion emulsion, by anti-
It should obtain low soap seed emulsion;
(3) by weight, by 10-30 parts of acrylic acid, 15-40 parts of styrene, 25-50 parts of methyl methacrylates and 5-
20 parts of butyl acrylates are mixed, agitated obtained third mix monomer lotion;
By weight, by the 5-25 parts of third mix monomer lotions, 0.01-0.015 parts of emulsifiers, 5-25 parts go from
Sub- water, 0.01-0.22 part redox type initiator and 0.1-0.7 parts of crosslinking agents are added to the 55-105 parts of low soap seed creams
In liquid, low soap core-shell emulsion is obtained after -65 DEG C of reactions 3-5 hours at 60 DEG C;
(4) by weight, the hydrogen for being 50% by the 70-75 parts of low soap core-shell emulsions and 5-8 parts of mass percentage concentrations
Oxidation aqueous solutions of potassium is mixed, and adds 1-5 parts into carbon auxiliary agent, 0.05-0.1 parts of ion fixatives, 0.01-0.05 parts of defoamings
Agent, 0.05-0.25 parts of plasticizer, 0.1-0.2 parts of levelling agents and 0.05-0.2 parts of curing agent, it is agitated, it stands, refilters, institute
Obtain the fire-resistant fluid that filtrate is composite fireproof glass.
Preferably, the polyalcohol is one or more of glycerol, xylitol and pentaerythrite.
Preferably, the function monomer be one or both of acrylic acid, methacrylic acid and polyacrylamide with
On.
Preferably, by weight, first mixed emulsion is by 15-20 parts of glycerol, 2-4 parts of xylitols, 2-4 parts of seasons
Penta tetrol, 10-15 part acrylic acid, 10-15 parts of methacrylic acids, 5-10 parts of polyacrylamides, 3-5 parts of boraxs, 3-5 parts of boric acid,
3-6 portions of sucrose, 0.1-0.2 parts of prodans and 10-15 parts of deionized waters are mixed to prepare.
Preferably, by weight, the second mix monomer lotion is by 15-20 parts of styrene, 20-30 parts of methyl
Methyl acrylate and 30-40 parts of butyl acrylates are mixed to prepare.
Preferably, by weight, the third mix monomer lotion is by 15-20 parts of acrylic acid, 20-30 parts of benzene second
Alkene, 30-40 part methyl methacrylate and 10-15 parts of butyl acrylates are mixed to prepare.
Preferably, the carbon forming agent is one or more of sucrose, fructose, glucose and granulated sugar;It is described at
Charcoal auxiliary agent is one or more of potassium dihydrogen phosphate, potassium hydrogen phosphate, sodium dihydrogen phosphate and dibastic sodium phosphate;The ion is solid
Determining agent is one or more of zinc oxide, aluminium oxide and starch;The defoaming agent is organic silicon modified by polyether and/or gathers
Urethane analog assistant;The plasticizer is dipropylene and/or dipropylene glycol methyl ether;The levelling agent is polyethers analog assistant;
The heat-resisting stabilizing agent is borax and/or boric acid;The curing agent be one of prodan, potassium fluosilicate and aluminum fluoride or
It is two or more;The crosslinking agent is 1,2- divinylbenzene;The redox type initiator is by ammonium persulfate and sulfurous acid
Hydrogen sodium is mixed with the molar ratio of 1:1;The emulsifier is by disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate and the poly- ethoxy of allyl
Base sulfonate is mixed with the mass ratio of 1:1;The granularity of the hydrophilic nano silica dioxide granule is 60nm-150nm.
On the other hand, the present invention provides a kind of fire-resistant fluid of composite fireproof glass, the fire prevention of the composite fireproof glass
Liquid is prepared by the preparation method of the fire-resistant fluid of above-mentioned composite fireproof glass.
Another aspect, the present invention provides a kind of composite fireproof glass, the composite fireproof glass include the first glass and
Fireproof gum made of second glass, first glass and second glass are solidified by fire-resistant fluid is combined layer by layer, institute
State the fire-resistant fluid that fire-resistant fluid is above-mentioned composite fireproof glass.
Preferably, second glass is laminated together by the fire prevention glue-line with third glass;First glass
The thickness of glass, second glass and the third glass is 4mm, and the thickness of the fire prevention glue-line is 1mm-2mm.
Compared with prior art, the beneficial effects of the present invention are:
The skill of the fire-resistant fluid of composite fireproof glass is prepared and mixing low soap core-shell emulsion and potassium hydroxide solution
Art means, solve composite fireproof glass fire-resistant fluid solidify made of fire prevention glue-line in there are microvesicle and the skills of fire protecting performance difference
Art problem has reached in the fire prevention glue-line of composite fireproof glass without microvesicle, the good technical effect of fire protecting performance.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of composite fireproof glass provided in an embodiment of the present invention;
Fig. 2 is the structural schematic diagram of another composite fireproof glass provided in an embodiment of the present invention.
Description of symbols:
1 first glass, 21 second glass, 3 fire prevention glue-lines, 22 third glass, 23 the 4th glass, 24 the 5th glass.
Specific embodiment
It is of the invention to reach the technical means and efficacy that predetermined goal of the invention is taken further to illustrate, below in conjunction with
Attached drawing is with preferred embodiment, to specific embodiment, technical solution, feature and its effect applied according to the present invention, specifically
It is bright as after.The special characteristic, structure or feature in multiple embodiments in following the description can be combined by any suitable form;This
When describing the preparation method of fire-resistant fluid of composite fireproof glass, used serial number (1) (2) (3) (4) does not limit this for invention
The step of inventive method, is sequentially;" one or more " that the present invention mentions, including the feelings by two kinds of material composition mixtures
Condition;In embodiment, for the allied substances with same or similar property and performance same effect, part of object is only enumerated
Matter is illustrated, and does not make all to enumerate, other unlisted substances, which equally have, has enumerated the had technical effect of substance;For
When the content of substance has range of choice, the partial data only enumerated in range of choice is illustrated, and is not made all to enumerate, be selected
Other unlisted data equally have technical effect possessed by enumerated data in range.
Embodiment 1
Accurately weigh first 0.15kg glycerol, 0.15kg acrylic acid, 0.02kg borax, 0.0005kg prodan,
0.02kg sucrose and 0.08kg deionized water, said components are mixed, and by being sufficiently stirred, the first mixed emulsion are made, for use;
Weigh above-mentioned first mixed emulsion of 0.3kg and 0.2kg partial size accurately as the hydrophilic nano silica of 60nm
Grain, passes through ultrasonic disperse for hydrophilic nano silica dioxide granule respectively and high-speed stirred is scattered in the first mixed emulsion, leads to
Crossing standing defoaming in 5 hours and forming weight is stable nanometer silicon dioxide particle dispersion emulsion, for use;
0.1kg styrene, 0.15kg methyl methacrylate and 0.2kg butyl acrylate accurately are weighed, by said components
By being sufficiently stirred the second mix monomer lotion is made, for use in mixing;
Disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate and allylpolyethoxy sulfonate are mixed according to mass ratio for 1:1
As the blended emulsifier of emulsion polymerization, and 0.1kg is prepared in advance, for use;
Ammonium persulfate and sodium hydrogensulfite are mixed with molar ratio for 1:1, and the redox as polymerization reaction
Type initiator, and it is stand-by to prepare 0.1kg in advance;
Accurately weigh the above-mentioned second mix monomer lotion of 0.01kg, the above-mentioned blended emulsifier of 0.0001kg, 0.001kg1,2-
Divinylbenzene and 0.05kg deionized water at the uniform velocity stir above-mentioned nanometer silicon dioxide particle dispersion with the revolving speed of 250rpm/min
Lotion, and be passed through nitrogen into above-mentioned nanometer silicon dioxide particle dispersion emulsion under stirring and protected, while stirring
Mix sequentially added under state into above-mentioned nanometer silicon dioxide particle dispersion emulsion the above-mentioned second mix monomer lotion of 0.01kg,
The above-mentioned blended emulsifier of 0.0001kg, 0.001kg1,2- divinylbenzene and 0.05kg deionized water, it is sufficiently mixed by stirring
It closes, stirs while slow heating is warming up to 60 DEG C, accurately weigh the redox type initiator that 0.0001kg is prepared in advance, then
The above-mentioned redox type initiator of 0.0001kg is added in above-mentioned nanometer silicon dioxide particle dispersion emulsion, in redox
Polymerization reaction occurs under conditions of type initiator and 60 DEG C of reaction temperatures, prepares low soap seed emulsion, for use;
Accurately weigh 0.1kg acrylic acid, 0.15kg styrene, 0.25kg methyl methacrylate and 0.05kg acrylic acid fourth
Ester mixes said components, by being sufficiently stirred, third mix monomer lotion is made, for use;
Accurately weigh the above-mentioned mixing cream of the above-mentioned third mix monomer lotion of 0.05kg, 0.05kg deionized water, 0.0001kg
The above-mentioned redox type initiator of agent, 0.0001kg and 0.001kg1,2- divinylbenzene, and be sufficiently mixed, it heats
To 60 DEG C, be added in above-mentioned low soap seed emulsion with constant speed, after completion of dropwise addition 60 DEG C isothermal reaction 4 hours, most
Low soap core-shell emulsion is obtained eventually;
Preparing weight in advance is the potassium hydroxide aqueous solution that 0.1kg mass fraction is 50%, and it is above-mentioned low accurately to weigh 0.7kg
The potassium hydroxide aqueous solution, 0.01kg potassium dihydrogen phosphate, 0.0005kg that soap core-shell emulsion, 0.05kg mass fraction are 50% form sediment
Powder, 0.0001kg organic silicon modified by polyether BYK-024,0.0005kg dipropylene, 0.001kg polyethers analog assistant RH-212
And 0.0005kg prodan;The potassium hydroxide for being first 50% by the above-mentioned low soap core-shell emulsion of 0.7kg and 0.05kg mass fraction
Aqueous solution is sufficiently mixed, and stir 10 minutes, sequentially add 0.01kg potassium dihydrogen phosphate, 0.0005kg starch,
0.0001kg organic silicon modified by polyether BYK-024,0.0005kg dipropylene, 0.001kg polyethers analog assistant RH-212 and
0.0005kg prodan, and stirred at low speed under the vacuum degree of 20mbar 20 minutes, holding is cooled to often under vacuum conditions
Wen Hou, then it is slowly increased to normal pressure, defoaming is stood under normal temperature and pressure, then by 100 mesh net filtrations, gained filtrate is compound anti-
The fire-resistant fluid of flint glass.
Embodiment 2
Accurately weigh first 0.2kg pentaerythrite, 0.2kg methacrylic acid, 0.04kg boric acid, 0.001kg potassium fluosilicate,
0.03kg fructose and 0.12kg deionized water, said components are mixed, and by being sufficiently stirred, the first mixed emulsion are made, for use;
Weigh above-mentioned first mixed emulsion of 0.32kg and 0.24kg partial size accurately as the hydrophilic nano silica of 80nm
Hydrophilic nano silica dioxide granule is passed through ultrasonic disperse respectively and high-speed stirred is scattered in the first mixed emulsion by particle,
It is stable nanometer silicon dioxide particle dispersion emulsion by standing defoaming in 6 hours to form weight, for use.
0.20kg styrene, 0.2kg methyl methacrylate and 0.3kg butyl acrylate accurately are weighed, by said components
By being sufficiently stirred the second mix monomer lotion is made, for use in mixing;
Disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate and allylpolyethoxy sulfonate are mixed according to mass ratio for 1:1
Blended emulsifier as emulsion polymerization.And it is stand-by to prepare 0.1kg in advance;
Ammonium persulfate and sodium hydrogensulfite are carried out mixing as the oxidation-reduction type of polymerization reaction for 1:1 using molar ratio to draw
Agent is sent out, and it is stand-by to prepare 0.1kg in advance;
The above-mentioned second mix monomer lotion of 0.03kg, the above-mentioned blended emulsifier of 0.00015kg, 0.002kg1 accurately are weighed,
2- divinylbenzene and 0.08kg deionized water at the uniform velocity stir above-mentioned nanometer silicon dioxide particle point with the revolving speed of 250rpm/min
Lotion is dissipated, and is passed through nitrogen into above-mentioned nanometer silicon dioxide particle dispersion emulsion under stirring and is protected, while
Sequentially added under stirring into above-mentioned nanometer silicon dioxide particle dispersion emulsion the above-mentioned second mix monomer lotion of 0.03kg,
The above-mentioned blended emulsifier of 0.00015kg, 0.002kg1,2- divinylbenzene and 0.08kg deionized water, it is sufficiently mixed by stirring
It closes, stirs while slow heating is warming up to 62 DEG C, accurately weigh the redox type initiator that 0.00015kg is prepared in advance,
The above-mentioned redox type initiator of 0.0002kg is added in above-mentioned nanometer silicon dioxide particle dispersion emulsion again, is gone back in oxidation
Polymerization reaction occurs under conditions of prototype initiator and reaction temperature, prepares low soap seed emulsion, for use.
Accurately weigh 0.15kg acrylic acid, 0.20kg styrene, 0.30kg methyl methacrylate and 0.10kg acrylic acid
Butyl ester mixes said components, by being sufficiently stirred, third mix monomer lotion is made, for use;
Accurately weigh the above-mentioned mixing cream of the above-mentioned third mix monomer lotion of 0.1kg, 0.08kg deionized water, 0.00011kg
The above-mentioned redox type initiator of agent, 0.0005kg and 0.002kg1,2- divinylbenzene, and be sufficiently mixed, it heats
To 62 DEG C, be added in above-mentioned low soap seed emulsion with constant speed, after completion of dropwise addition 62 DEG C isothermal reaction 4 hours, most
Low soap core-shell emulsion is obtained eventually.
Preparing weight in advance is the potassium hydroxide aqueous solution that 0.1kg mass fraction is 50%, and it is above-mentioned accurately to weigh 0.71kg
Potassium hydroxide aqueous solution, 0.02kg potassium hydrogen phosphate, the 0.0006kg oxidation that low soap core-shell emulsion, 0.06kg mass fraction are 50%
Zinc, 0.0002kg polyurethanes auxiliary agent 902W, 0.001kg dipropylene glycol methyl ether, 0.002kg polyethers analog assistant RH-212 and
0.0008kg prodan;The potassium hydroxide water for being first 50% by the above-mentioned low soap core-shell emulsion of 0.71kg and 0.06kg mass fraction
Solution is sufficiently mixed, and stir 10 minutes, sequentially add 0.02kg potassium hydrogen phosphate, 0.0006kg zinc oxide,
0.0002kg polyurethanes auxiliary agent 902W, 0.001kg dipropylene glycol methyl ether, 0.002kg polyethers analog assistant RH-212 and
0.0008kg prodan, and stirred at low speed under the vacuum degree of 25mbar 20 minutes, it is maintained at vacuum state and is cooled to room temperature
Afterwards, then it is slowly increased to normal pressure, defoaming is stood under normal temperature and pressure, then by 100 mesh net filtrations, gained filtrate is composite fire-proof
The fire-resistant fluid of glass.
Embodiment 3
Accurately weigh first 0.23kg xylitol, 0.25kg polyacrylamide, 0.03kg borax and 0.03kg boric acid,
0.0015kg aluminum fluoride, 0.04kg glucose and 0.16kg deionized water, said components are mixed, and by being sufficiently stirred, are made
First mixed emulsion, for use;
The hydrophilic nano silica that above-mentioned first mixed emulsion of accurate measuring 0.34kg and 0.28kg partial size are 100nm
Hydrophilic nano silica dioxide granule is passed through ultrasonic disperse respectively and high-speed stirred is scattered in the first mixed emulsion by particle,
It is stable nanometer silicon dioxide particle dispersion emulsion by standing defoaming in 7 hours to form weight, for use.
0.20kg styrene, 0.25kg methyl methacrylate and 0.35kg butyl acrylate accurately are weighed, by above-mentioned group
Divide mixing, by being sufficiently stirred, the second mix monomer lotion is made, for use;
Disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate and allylpolyethoxy sulfonate are mixed according to mass ratio for 1:1
Blended emulsifier as emulsion polymerization.And it is stand-by to prepare 0.1kg in advance;
Ammonium persulfate and sodium hydrogensulfite are carried out mixing as the oxidation-reduction type of polymerization reaction for 1:1 using molar ratio to draw
Agent is sent out, and it is stand-by to prepare 0.1kg in advance;
Accurately weigh the above-mentioned second mix monomer lotion of 0.05kg, the above-mentioned blended emulsifier of 0.0002kg, 0.003kg1,2-
Divinylbenzene and 0.08kg deionized water at the uniform velocity stir above-mentioned nanometer silicon dioxide particle dispersion with the revolving speed of 250rpm/min
Lotion, and be passed through nitrogen into above-mentioned nanometer silicon dioxide particle dispersion emulsion under stirring and protected, while stirring
Mix sequentially added under state into above-mentioned nanometer silicon dioxide particle dispersion emulsion the above-mentioned second mix monomer lotion of 0.05kg,
The above-mentioned blended emulsifier of 0.0002kg, 0.003kg1,2- divinylbenzene and 0.08kg deionized water, it is sufficiently mixed by stirring
It closes, stirs while slow heating is warming up to 63 DEG C, accurately weigh the redox type initiator that 0.0003kg is prepared in advance, then
The above-mentioned redox type initiator of 0.0003kg is added in above-mentioned nanometer silicon dioxide particle dispersion emulsion, in redox
Polymerization reaction occurs under conditions of type initiator and reaction temperature, prepares low soap seed emulsion, for use.
Accurately weigh 0.20kg acrylic acid, 0.25kg styrene, 0.35kg methyl methacrylate and 0.15kg acrylic acid
Butyl ester mixes said components, by being sufficiently stirred, third mix monomer lotion is made, for use;
Accurately weigh the above-mentioned mixing cream of the above-mentioned third mix monomer lotion of 0.15kg, 0.08kg deionized water, 0.00012kg
The above-mentioned redox type initiator of agent, 0.001kg and 0.003kg1,2- divinylbenzene, and be sufficiently mixed, it is heated to
63 DEG C, be added in above-mentioned low soap seed emulsion with constant speed, after completion of dropwise addition 63 DEG C isothermal reaction 4 hours, finally
Obtain low soap core-shell emulsion.
Preparing weight in advance is the potassium hydroxide aqueous solution that 0.1kg mass fraction is 50%, and it is above-mentioned accurately to weigh 0.72kg
Low soap core-shell emulsion, the potassium hydroxide aqueous solution that 0.07kg mass fraction is 50%, 0.03kg sodium dihydrogen phosphate, 0.0014kg oxygen
Change aluminium, 0.0003kg polyurethanes auxiliary agent 902W, 0.0007kg dipropylene and 0.0007kg dipropylene glycol methyl ether,
0.0014kg polyethers analog assistant RH-212 and 0.0012kg aluminum fluoride;First by the above-mentioned low soap core-shell emulsion of 0.72kg and 0.07kg matter
The potassium hydroxide aqueous solution that amount score is 50% is sufficiently mixed, and is stirred 10 minutes, and 0.03kg di(2-ethylhexyl)phosphate is sequentially added
Hydrogen sodium, 0.0007kg aluminium oxide, 0.0003kg polyurethanes auxiliary agent 902W, 0.0007kg dipropylene and 0.0007kg bis-
Propylene glycol monomethyl ether, 0.0014kg polyethers analog assistant RH-212 and 0.0012kg aluminum fluoride, and the low speed under the vacuum degree of 30mbar
Stirring 20 minutes is maintained at after vacuum state is cooled to room temperature, then is slowly increased to normal pressure, defoaming is stood under normal temperature and pressure, then lead to
Net filtration is sieved with 100 mesh sieve, gained filtrate is the fire-resistant fluid of composite fireproof glass.
Embodiment 4
Accurately weigh first 0.2kg glycerol and 0.05kg pentaerythrite, 0.15kg acrylic acid and 0.15kg methacrylic acid,
0.04kg borax and 0.04kg boric acid, 0.001kg prodan and 0.001kg potassium fluosilicate, 0.05kg granulated sugar and 0.18kg are gone
Ionized water mixes said components, by being sufficiently stirred, the first mixed emulsion is made, for use;
Weigh above-mentioned first mixed emulsion of 0.36kg and 0.32kg partial size accurately as the hydrophilic nano silica of 120nm
Hydrophilic nano silica dioxide granule is passed through ultrasonic disperse respectively and high-speed stirred is scattered in the first mixed emulsion by particle,
It is stable nanometer silicon dioxide particle dispersion emulsion by standing defoaming in 8 hours to form weight, for use.
0.25kg styrene, 0.30kg methyl methacrylate and 0.40kg butyl acrylate accurately are weighed, by above-mentioned group
Divide mixing, by being sufficiently stirred, the second mix monomer lotion is made, for use;
Disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate and allylpolyethoxy sulfonate are mixed according to mass ratio for 1:1
Blended emulsifier as emulsion polymerization.And it is stand-by to prepare 0.1kg in advance;
Ammonium persulfate and sodium hydrogensulfite are carried out mixing as the oxidation-reduction type of polymerization reaction for 1:1 using molar ratio to draw
Agent is sent out, and it is stand-by to prepare 0.1kg in advance;
The above-mentioned second mix monomer lotion of 0.08kg, the above-mentioned blended emulsifier of 0.00025kg, 0.005kg1 accurately are weighed,
2- divinylbenzene and 0.11kg deionized water at the uniform velocity stir above-mentioned nanometer silicon dioxide particle point with the revolving speed of 250rpm/min
Lotion is dissipated, and is passed through nitrogen into above-mentioned nanometer silicon dioxide particle dispersion emulsion under stirring and is protected, while
Sequentially added under stirring into above-mentioned nanometer silicon dioxide particle dispersion emulsion the above-mentioned second mix monomer lotion of 0.08kg,
The above-mentioned blended emulsifier of 0.00025kg, 0.005kg1,2- divinylbenzene and 0.11kg deionized water, it is sufficiently mixed by stirring
It closes, stirs while slow heating is warming up to 64 DEG C, accurately weigh the redox type initiator that 0.0004kg is prepared in advance, then
The above-mentioned redox type initiator of 0.0004kg is added in above-mentioned nanometer silicon dioxide particle dispersion emulsion, in redox
Polymerization reaction occurs under conditions of type initiator and reaction temperature, prepares low soap seed emulsion, for use.
Accurately weigh 0.25kg acrylic acid, 0.30kg styrene, 0.40kg methyl methacrylate and 0.20kg acrylic acid
Butyl ester mixes said components, by being sufficiently stirred, third mix monomer lotion is made, for use;
Accurately weigh the above-mentioned mixing cream of the above-mentioned third mix monomer lotion of 0.2kg, 0.12kg deionized water, 0.00013kg
The above-mentioned redox type initiator of agent, 0.0015kg and 0.005kg1,2- divinylbenzene, and be sufficiently mixed, it heats
To 64 DEG C, be added in above-mentioned low soap seed emulsion with constant speed, after completion of dropwise addition 64 DEG C isothermal reaction 4 hours, most
Low soap core-shell emulsion is obtained eventually.
Preparing weight in advance is the potassium hydroxide aqueous solution that 0.1kg mass fraction is 50%, and it is above-mentioned accurately to weigh 0.73kg
Potassium hydroxide aqueous solution, 0.04kg dibastic sodium phosphate, the 0.0004kg oxidation that low soap core-shell emulsion, 0.08kg mass fraction are 50%
Aluminium and 0.0004kg starch, 0.0002kg organic silicon modified by polyether BYK-024 and 0.0002kg polyurethanes auxiliary agent 902W,
0.0008kg dipropylene and 0.0008kg dipropylene glycol methyl ether, 0.0016kg polyethers analog assistant RH-212 and 0.0008kg
Aluminum fluoride and 0.0008kg prodan;The hydrogen for being first 50% by the above-mentioned low soap core-shell emulsion of 0.73kg and 0.08kg mass fraction
Oxidation aqueous solutions of potassium is sufficiently mixed, and is stirred 10 minutes, and 0.04kg sodium dihydrogen phosphate, 0.0004kg oxidation are sequentially added
Aluminium and 0.0004kg starch, 0.0002kg organic silicon modified by polyether BYK-024 and 0.0002kg polyurethanes auxiliary agent 902W,
0.0008kg dipropylene and 0.0008kg dipropylene glycol methyl ether, 0.0016kg polyethers analog assistant RH-212 and 0.0008kg
Aluminum fluoride and 0.0008kg prodan, and stirred at low speed under the vacuum degree of 35mbar 20 minutes, it is cold to be maintained at vacuum state
But to after room temperature, then it is slowly increased to normal pressure, defoaming is stood under normal temperature and pressure, then by 100 mesh net filtrations, gained filtrate is
The fire-resistant fluid of composite fireproof glass.
Embodiment 5
0.24kg glycerol and 0.04kg xylitol, 0.18kg polyacrylamide and 0.17kg metering system are accurately weighed first
Acid, 0.05kg borax and 0.05kg boric acid, 0.0012kg prodan and 0.0013kg aluminum fluoride, 0.03kg sucrose and 0.03kg
Fructose and 0.2kg deionized water, said components are mixed, and by being sufficiently stirred, the first mixed emulsion are made, for use;
Weigh above-mentioned first mixed emulsion of 0.38kg and 0.36kg partial size accurately as the hydrophilic nano silica of 140nm
Hydrophilic nano silica dioxide granule is passed through ultrasonic disperse respectively and high-speed stirred is scattered in the first mixed emulsion by particle,
It is stable nanometer silicon dioxide particle dispersion emulsion by standing defoaming in 9 hours to form weight, for use.
0.3kg styrene, 0.35kg methyl methacrylate and 0.45kg butyl acrylate accurately are weighed, by said components
By being sufficiently stirred the second mix monomer lotion is made, for use in mixing;
Disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate and allylpolyethoxy sulfonate are mixed according to mass ratio for 1:1
Blended emulsifier as emulsion polymerization.And it is stand-by to prepare 0.1kg in advance;
Ammonium persulfate and sodium hydrogensulfite are carried out mixing as the oxidation-reduction type of polymerization reaction for 1:1 using molar ratio to draw
Agent is sent out, and it is stand-by to prepare 0.1kg in advance;
The above-mentioned second mix monomer lotion of accurate measuring 0.07kg, the above-mentioned blended emulsifier of 0.00022kg, 0.007kg1,
2- divinylbenzene and 0.15kg deionized water at the uniform velocity stir above-mentioned nanometer silicon dioxide particle point with the revolving speed of 250rpm/min
Lotion is dissipated, and is passed through nitrogen into above-mentioned nanometer silicon dioxide particle dispersion emulsion under stirring and is protected, while
Sequentially added under stirring into above-mentioned nanometer silicon dioxide particle dispersion emulsion the above-mentioned second mix monomer lotion of 0.07kg,
The above-mentioned blended emulsifier of 0.00022kg, 0.007kg1,2- divinylbenzene and 0.15kg deionized water, it is sufficiently mixed by stirring
It closes, stirs while slow heating is warming up to 65 DEG C, accurately weigh the redox type initiator that 0.00025kg is prepared in advance,
The above-mentioned redox type initiator of 0.0005kg is added in above-mentioned nanometer silicon dioxide particle dispersion emulsion again, is gone back in oxidation
Polymerization reaction occurs under conditions of prototype initiator and reaction temperature, prepares low soap seed emulsion, for use.
Accurately weigh 0.3kg acrylic acid, 0.35kg styrene, 0.45kg methyl methacrylate and 0.20kg acrylic acid fourth
Ester mixes said components, by being sufficiently stirred, third mix monomer lotion is made, for use;
Accurately weigh the above-mentioned mixing cream of the above-mentioned third mix monomer lotion of 0.25kg, 0.15kg deionized water, 0.00014kg
The above-mentioned redox type initiator of agent, 0.002kg and 0.007kg1,2- divinylbenzene, and be sufficiently mixed, it is heated to
65 DEG C, be added in above-mentioned low soap seed emulsion with constant speed, after completion of dropwise addition 65 DEG C isothermal reaction 4 hours, finally
Obtain low soap core-shell emulsion.
Preparing weight in advance is the potassium hydroxide aqueous solution that 0.1kg mass fraction is 50%, and it is above-mentioned accurately to weigh 0.74kg
Low soap core-shell emulsion, potassium hydroxide aqueous solution, 0.025kg potassium hydrogen phosphate and the 0.025kg phosphorus that 0.065kg mass fraction is 50%
Acid dihydride potassium, 0.00045kg zinc oxide and 0.00045kg starch, 0.0003kg organic silicon modified by polyether BYK-024 and
0.0002kg polyurethanes auxiliary agent 902W, 0.0018kg dipropylene, 0.0018kg polyethers analog assistant RH-212 and
0.0009kg aluminum fluoride and 0.0009kg potassium fluosilicate;First by the above-mentioned low soap core-shell emulsion of 0.74kg and 0.065kg mass fraction
Be sufficiently mixed for 50% potassium hydroxide aqueous solution, and stir 10 minutes, sequentially add 0.025kg potassium hydrogen phosphate and
0.025kg potassium dihydrogen phosphate, 0.00045kg zinc oxide and 0.00045kg starch, 0.0003kg organic silicon modified by polyether BYK-
024 and 0.0002kg polyurethanes auxiliary agent 902W, 0.0018kg dipropylene, 0.0018kg polyethers analog assistant RH-212 and
0.0009kg aluminum fluoride and 0.0009kg potassium fluosilicate, and stirred at low speed under the vacuum degree of 40mbar 20 minutes, it is maintained at true
After dummy status is cooled to room temperature, then it is slowly increased to normal pressure, defoaming is stood under normal temperature and pressure, then pass through 100 mesh net filtrations, gained
Filtrate is the fire-resistant fluid of composite fireproof glass.
Embodiment 6
0.15kg pentaerythrite and 0.16kg xylitol, 0.2kg polyacrylamide and 0.2kg propylene are accurately weighed first
Acid, 0.06kg borax and 0.06kg boric acid, 0.0015kg prodan and 0.0015kg potassium fluosilicate, 0.04kg glucose and
0.03kg granulated sugar and 0.17kg deionized water, said components are mixed, and by being sufficiently stirred, the first mixed emulsion are made, for use;
Weigh above-mentioned first mixed emulsion of 0.4kg and 0.4kg partial size accurately as the hydrophilic nano silica of 150nm
Grain, passes through ultrasonic disperse for hydrophilic nano silica dioxide granule respectively and high-speed stirred is scattered in the first mixed emulsion, leads to
Crossing standing defoaming in 9 hours and forming weight is stable nanometer silicon dioxide particle dispersion emulsion, for use.
0.28kg styrene, 0.40kg methyl methacrylate and 0.50kg butyl acrylate accurately are weighed, by above-mentioned group
Divide mixing, by being sufficiently stirred, the second mix monomer lotion is made, for use;
Disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate and allylpolyethoxy sulfonate are mixed according to mass ratio for 1:1
Blended emulsifier as emulsion polymerization.And it is stand-by to prepare 0.1kg in advance;
Ammonium persulfate and sodium hydrogensulfite are carried out mixing as the oxidation-reduction type of polymerization reaction for 1:1 using molar ratio to draw
Agent is sent out, and it is stand-by to prepare 0.1kg in advance;
The above-mentioned second mix monomer lotion of 0.08kg, the above-mentioned blended emulsifier of 0.00018kg, 0.007kg1 accurately are weighed,
2- divinylbenzene and 0.15kg deionized water at the uniform velocity stir above-mentioned nanometer silicon dioxide particle point with the revolving speed of 250rpm/min
Lotion is dissipated, and is passed through nitrogen into above-mentioned nanometer silicon dioxide particle dispersion emulsion under stirring and is protected, while
Sequentially added under stirring into above-mentioned nanometer silicon dioxide particle dispersion emulsion the above-mentioned second mix monomer lotion of 0.08kg,
The above-mentioned blended emulsifier of 0.00018kg, 0.007kg1,2- divinylbenzene and 0.15kg deionized water, it is sufficiently mixed by stirring
It closes, stirs while slow heating is warming up to 65 DEG C, accurately weigh the redox type initiator that 0.00025kg is prepared in advance,
The above-mentioned redox type initiator of 0.00045kg is added in above-mentioned nanometer silicon dioxide particle dispersion emulsion again, is being aoxidized
Polymerization reaction occurs under conditions of reduced form initiator and reaction temperature, prepares low soap seed emulsion, for use.
Accurately weigh 0.3kg acrylic acid, 0.35kg styrene, 0.45kg methyl methacrylate and 0.20kg acrylic acid fourth
Ester mixes said components, by being sufficiently stirred, third mix monomer lotion is made, for use;
Accurately weigh the above-mentioned mixing cream of the above-mentioned third mix monomer lotion of 0.25kg, 0.25kg deionized water, 0.00015kg
The above-mentioned redox type initiator of agent, 0.0022kg and 0.007kg1,2- divinylbenzene, and be sufficiently mixed, it heats
To 65 DEG C, be added in above-mentioned low soap seed emulsion with constant speed, after completion of dropwise addition 65 DEG C isothermal reaction 4 hours, most
Low soap core-shell emulsion is obtained eventually.
Preparing weight in advance is the potassium hydroxide aqueous solution that 0.1kg mass fraction is 50%, and it is above-mentioned accurately to weigh 0.75kg
Low soap core-shell emulsion, potassium hydroxide aqueous solution, 0.020kg potassium hydrogen phosphate and the 0.020kg phosphorus that 0.075kg mass fraction is 50%
Acid dihydride potassium and 0.01kg dibastic sodium phosphate, 0.00035kg zinc oxide and 0.00035kg starch and aluminium oxide, 0.0003kg polyethers
Modified organic silicon BYK-024 and 0.0002kg polyurethanes auxiliary agent 902W, 0.0025kg dipropylene, 0.002kg polyethers
Analog assistant RH-212 and 0.0006kg aluminum fluoride and 0.0007kg potassium fluosilicate and 0.0007kg prodan;It first will be on 0.75kg
It states the potassium hydroxide aqueous solution that low soap core-shell emulsion and 0.055kg mass fraction are 50% to be sufficiently mixed, and stirs 10 points
Clock sequentially adds 0.020kg potassium hydrogen phosphate and 0.020kg potassium dihydrogen phosphate and 0.01kg dibastic sodium phosphate, 0.00035kg oxidation
Zinc and 0.00035kg starch and aluminium oxide, 0.0003kg organic silicon modified by polyether BYK-024 and 0.0002kg polyurethanes auxiliary agent
902W, 0.0025kg dipropylene, 0.002kg polyethers analog assistant RH-212 and 0.0006kg aluminum fluoride and 0.0007kg fluorine
Potassium silicate and 0.0007kg prodan, and stirred at low speed under the vacuum degree of 35mbar 20 minutes, it is cold to be maintained at vacuum state
But to after room temperature, then it is slowly increased to normal pressure, defoaming is stood under normal temperature and pressure, then by 100 mesh net filtrations, gained filtrate is
The fire-resistant fluid of composite fireproof glass.
Embodiment 7
Accurately weigh first 0.18kg glycerol and 0.03kg pentaerythrite and 0.03kg xylitol, 0.13kg acrylic acid and
0.13kg methacrylic acid and 0.07kg polyacrylamide, 0.045kg borax and 0.045kg boric acid, 0.0005kg prodan
With 0.0005kg potassium fluosilicate and 0.0005kg aluminum fluoride, 0.015kg sucrose and 0.015kg fructose and 0.01kg glucose and
0.005kg granulated sugar and 0.13kg deionized water, said components are mixed, by being sufficiently stirred, obtained first mixed emulsion, to
With;
Weigh above-mentioned first mixed emulsion of 0.35kg and 0.3kg partial size accurately as the hydrophilic nano silica of 105nm
Hydrophilic nano silica dioxide granule is passed through ultrasonic disperse respectively and high-speed stirred is scattered in the first mixed emulsion by particle,
It is stable nanometer silicon dioxide particle dispersion emulsion by standing defoaming in 7.5 hours to form weight, for use.
0.275kg styrene, 0.35kg methyl methacrylate and 0.35kg butyl acrylate accurately are weighed, by above-mentioned group
Divide mixing, by being sufficiently stirred, the second mix monomer lotion is made, for use;
Disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate and allylpolyethoxy sulfonate are mixed according to mass ratio for 1:1
Blended emulsifier as emulsion polymerization.And it is stand-by to prepare 0.1kg in advance;
Ammonium persulfate and sodium hydrogensulfite are carried out mixing as the oxidation-reduction type of polymerization reaction for 1:1 using molar ratio to draw
Agent is sent out, and it is stand-by to prepare 0.1kg in advance;
Accurately weigh the above-mentioned second mix monomer lotion of 0.035kg, the above-mentioned blended emulsifier of 0.000155kg,
0.0035kg1,2- divinylbenzene and 0.15kg deionized water at the uniform velocity stir above-mentioned nano-silica with the revolving speed of 250rpm/min
Silicon carbide particle dispersion emulsion, and be passed through nitrogen into above-mentioned nanometer silicon dioxide particle dispersion emulsion under stirring and protected
Shield, while sequentially adding 0.035kg above-mentioned second into above-mentioned nanometer silicon dioxide particle dispersion emulsion under stirring and mixing
Monomer emulsions, the above-mentioned blended emulsifier of 0.000155kg, 0.0035kg1,2- divinylbenzene and 0.075kg deionized water are closed,
It is sufficiently mixed by stirring, stirs while slow heating is warming up to 63 DEG C, accurately weigh the oxidation that 0.00025kg is prepared in advance
Reduced form initiator, then the above-mentioned redox type initiator of 0.00025kg is added to above-mentioned nanometer silicon dioxide particle and is dispersed
In lotion, polymerization reaction occurs under conditions of redox type initiator and reaction temperature, prepares low soap seed emulsion, to
With.
Accurately weigh 0.175kg acrylic acid, 0.25kg styrene, 0.35kg methyl methacrylate and 0.125kg propylene
Acid butyl ester mixes said components, by being sufficiently stirred, third mix monomer lotion is made, for use;
Accurately weigh the above-mentioned mixing cream of the above-mentioned third mix monomer lotion of 0.15kg, 0.20kg deionized water, 0.00015kg
The above-mentioned redox type initiator of agent, 0.00017kg and 0.0035kg1,2- divinylbenzene, and be sufficiently mixed, add
Heat is added in above-mentioned low soap seed emulsion to 63 DEG C with constant speed, after completion of dropwise addition 63 DEG C isothermal reaction 4 hours,
Finally obtain low soap core-shell emulsion.
Preparing weight in advance is the potassium hydroxide aqueous solution that 0.1kg mass fraction is 50%, and it is above-mentioned accurately to weigh 0.725kg
Low soap core-shell emulsion, potassium hydroxide aqueous solution, 0.01kg potassium hydrogen phosphate and the 0.010kg phosphorus that 0.065kg mass fraction is 50%
Acid dihydride potassium and 0.01kg dibastic sodium phosphate and 0.005kg sodium dihydrogen phosphate, 0.0003kg zinc oxide and 0.0003kg starch and
0.0002kg aluminium oxide, 0.00015kg organic silicon modified by polyether BYK-024 and 0.00015kg polyurethanes auxiliary agent 902W,
0.0020kg dipropylene glycol methyl ether, 0.0015kg polyethers analog assistant RH-212 and 0.0005kg aluminum fluoride and 0.0005kg fluosilicic acid
Potassium and 0.0005kg prodan;The hydrogen-oxygen for being first 50% by the above-mentioned low soap core-shell emulsion of 0.725kg and 0.065kg mass fraction
Change aqueous solutions of potassium to be sufficiently mixed, and stir 10 minutes, sequentially adds 0.01kg potassium hydrogen phosphate and 0.010kg biphosphate
Potassium and 0.01kg dibastic sodium phosphate and 0.005kg sodium dihydrogen phosphate, 0.0003kg zinc oxide and 0.0003kg starch and 0.0002kg
Aluminium oxide, 0.00015kg organic silicon modified by polyether and 0.00015kg polyurethanes auxiliary agent 902W, 0.0020kg dipropylene glycol first
Ether, 0.0015kg polyethers analog assistant RH-212 and 0.0005kg aluminum fluoride and 0.0005kg potassium fluosilicate and 0.0005kg fluosilicic acid
Sodium, and stirring at low speed under the vacuum degree of 30mbar 20 minutes is maintained at after vacuum state is cooled to room temperature, then is slowly increased to often
It presses, defoaming is stood under normal temperature and pressure, then by 100 mesh net filtrations, gained filtrate is the fire-resistant fluid of composite fireproof glass.
The effect of each auxiliary agent is as follows in the fire-resistant fluid of above-mentioned composite fireproof glass:
Polyalcohol: refer in molecule containing there are three or three or more hydroxyls alcohols, such as glycerol, trihydroxy methyl ethane,
Pentaerythrite, xylitol, sorbierite etc.;It is all that there is stronger crystallinity and can be used compared with the polyalcohol of high bond strength;This
The polyalcohol that uses is invented as one or more of glycerol, xylitol and pentaerythrite, by using above-mentioned polyalcohol,
Improve the cohesiveness and intensity of composite fireproof glass;Above-mentioned polyalcohol is also hydrocarbon simultaneously, also can be used as carbon forming agent,
Have the function of surfactant to a certain extent, and itself plays certain defoaming and antifreezing effect.
Function monomer: the monomer of specific function group can be provided by referring to, such as cohesiveness, water resistance, stability;It is all to mention
The cohesiveness of the fire-resistant fluid of high composite fireproof glass and the function monomer of stability can be used;The function monomer that the present invention uses
For one or more of acrylic acid, methacrylic acid and polyacrylamide;Wherein, acrylic acid and methacrylic acid conduct
Water-soluble monomer, can be used as emulsifier, synthetic polymer monomer, methyl methacrylate and styrene as comonomer, can
The glass transition temperature for adjusting each one polymer of the fire-resistant fluid of composite fireproof glass, increases its adhesion strength and stability.
Carbon forming agent and at charcoal auxiliary agent: under enough heats, the hydroxyl in molecule is broken from carbochain, loses the carbon of hydroxyl
The Viability charcoal of chain, active carbon form insulating layer to prevent hot transmitting;It is all can be formed at high temperature long-chain charcoal insulating layer at
Charcoal agent can be used;The carbon forming agent that the present invention uses for one or more of sucrose, fructose, glucose and granulated sugar, at
Carbon auxiliary agent is one or more of potassium dihydrogen phosphate, potassium hydrogen phosphate, sodium dihydrogen phosphate and dibastic sodium phosphate;When fire prevention glue-line
When foaming generates hole at high temperature, carbon forming agent and the carbide to form long-chain is carbonized at charcoal auxiliary agent, be deposited in above-mentioned hole,
The carbide of long-chain can absorb amount of heat, to enhance the fire protecting performance of glass.
Defoaming agent: can inhibit generation foam or eliminate the foam generated;The defoaming agent that the present invention uses is polyether-modified
Organosilicon BYK-024 and/or polyurethanes auxiliary agent 902W;Due to needing to stir just in the fire-resistant fluid for preparing composite fireproof glass
Each substance can be made to be sufficiently mixed, and stir and inevitably generate bubble simultaneously, be solidified into the fire-resistant fluid of composite fireproof glass
Fireproof gum and when being overlying on the surface of composite fireproof glass, bubble can be present in fire prevention glue-line, make the apparent of composite fireproof glass
Quality becomes poor, and can eliminate the bubble in fire-resistant fluid by the way that above-mentioned defoaming agent is added, that is, eliminates the gas in fire prevention glue-line
Bubble, and then improve the apparent mass of composite fireproof glass.Heat-resisting stabilizing agent: the heat-resisting stabilizing agent that the present invention uses is borax
And/or boric acid, there is anti-flammability, the heat-resisting and transparent of glue-line of preventing fires that the fire-resistant fluid of composite fireproof glass is solidified into can be improved
Can, the coefficient of thermal expansion of above-mentioned fire prevention glue-line is controlled, and then improve chemical stability, the resistance to mechanical impact capacity of composite fireproof glass
And thermal shock ability.
Ion fixative: the ion fixative that the present invention uses is one or both of zinc oxide, aluminium oxide and starch
More than, the activity of potassium oxide, above-mentioned by being added in the fire prevention glue-line that the fire-resistant fluid of changeable composite fireproof glass is solidified into
The water resistance of above-mentioned fire prevention glue-line can be improved in ion fixative.
Levelling agent: the levelling agent that the present invention uses overlays on for polyethers analog assistant RH-212 when preparing composite fireproof glass
The fire-resistant fluid coating needs of the composite fireproof glass on composite fireproof glass surface dry, since composite fireproof glass has centainly
Amount of deflection, in dry process, it is poor that the fire prevention glue-line that the fire-resistant fluid of composite fireproof glass is solidified into inevitably generates thickness, leads to
It crosses and above-mentioned levelling agent is added, above-mentioned fire prevention glue-line is made to remain to form smooth, smooth and uniform glue-line after compression, on guaranteeing
It states and prevents fires glue-line uniformly and bubble-free.
Curing agent: the curing agent that the present invention uses be one or both of prodan, potassium fluosilicate and aluminum fluoride with
On, the fire-resistant fluid of low soap core-shell emulsion and potassium hydroxide aqueous solution reaction generation composite fireproof glass, the i.e. higher potassium of solid content
Waterglass, can accelerate the reaction speed and curing rate of the two using curing agent, and the fire-resistant fluid for improving composite fireproof glass is solid
The intensity of the fire prevention glue-line of chemical conversion and the intensity of composite fireproof glass.
Crosslinking agent: the crosslinking agent that the present invention uses can accelerate the fire prevention of composite fireproof glass for 1,2- divinylbenzene
The hardening of liquid improves the heat resistance of the fire-resistant fluid of composite fireproof glass, improves fireproof gum made of composite fireproof glass solidifies
Mechanical strength and weatherability.
Plasticizer: the plasticizer that the present invention uses is dipropylene and/or dipropylene glycol methyl ether, can be reduced compound anti-
The glass transition temperature of fireproof gum made of the fire-resistant fluid of flint glass solidifies enhances the toughness, plasticity and cohesiveness of above-mentioned fireproof gum,
The impact strength for improving above-mentioned fireproof gum accelerates the curing rate of the fire-resistant fluid of composite fireproof glass.
Initiator: the present invention use using molar ratio for 1:1 ammonium persulfate and sodium hydrogensulfite mixture as oxidation
Initiator is restored, monomer can be caused and carry out polymerization reaction, be to prepare the important component part of above-mentioned low soap core-shell emulsion, directly
Influence the polymerization rate of above-mentioned low soap core-shell emulsion, the conversion ratio of monomer and particle size of final particle etc.;Oxidation
Restoring initiator system is to cause low neat soap shell using the electronics transfer free radical generated between Oxidizing and Reducing Agents
The polymerization reaction of lotion, since the reaction activity of redox initiation system is much smaller than the reaction activity of hot initiator system,
The initiation temperature of above-mentioned low soap core-shell emulsion can be reduced, reaction rate is improved, reduces energy consumption of reaction, while portion can also be avoided
Divide the generation hydrolysis of function monomer at high temperature.
Emulsifier: the fire-resistant fluid of composite fireproof glass of the invention is low soap lotion: containing micro emulsification i.e. in lotion
Agent not only saves cost, also improves emulsion intercalation method;Emulsifier has good divergent function, in molecule simultaneously
It with hydrophilic group and lipophilic group, and is gathered on oil-water interfaces, stable dispersion can be formed;The emulsifier that the present invention uses
It is mixed by disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate and allylpolyethoxy sulfonate according to mass ratio for 1:1, entire
During emulsion polymerization, the parts by weight of addition only have 0.01-0.025, and the emulsifier of addition can reduce interfacial tension
Energy required for lotion is formed with reduction, promotes the dispersion of liquid in a liquid, prepares W/O emulsification system, it is steady to improve product
It is qualitative;When the present invention prepares stable emulsion system, certain stable emulsion dispersion is played in addition to adding micro emulsifier
The effect of system, there are also acrylic acid can also play the role of similar emulsifier, i.e. promotion lotion forms stable dispersion, because
It is water-soluble monomer for acrylic acid, not only contains hydrophilic radical-COOH, but also contain hydrophobic grouping-CH3, therefore in this hair
In bright low soap emulsion polymerization, a part of acrylic monomers approximate can also play the role of emulsifier, and another part propylene
Acid can play the role of polymerized monomer again, while the glass transition temperature of acrylic acid is 105 degree or so, with styrene, first
Base methyl acrylate is similar.
The fire-resistant fluid of the composite fireproof glass of the method for the present invention preparation is the lotion of core-shell structure: being primarily referred to as two kinds or more
Kind of monomer stage by stage or multi-stage polymeric, makes the inner or outer side of emulsion particle be enriched with heterogeneity, i.e. core respectively under certain condition
Shell mould emulsion particle obtains the multiple emulsion of different performance to impart core and the variant function of shell.
When preparing the second mix monomer lotion in the method for the present invention, styrene, methyl methacrylate and acrylic acid are used
Butyl ester carries out reaction and obtains copolymer, and styrene is due to containing phenyl ring, and its glass transition temperature is 105 degree or so, at normal temperature
For glassy state, the rigidity of copolymer can be improved, simultaneously because 2- divinylbenzene is crosslinking agent, it is easy to make benzene second using 1
Alkene and other monomers are copolymerized, and the glass transition temperature of polymethyl methacrylate is similar to polystyrene, is not influencing copolymer
Under the premise of glass transition temperature, cost can be reduced;The glass transition temperature of butyl acrylate be -56 degree left and right, at normal temperature for
Rubbery state can be improved the toughness of copolymer, prevent copolymer from brittle fracture occurring in use.According to the method for the present invention
In the obtained copolymer of component proportion, i.e. the second mix monomer lotion can according to the glass transition temperature formula calculating of copolymer
Know, the glass transition temperature of the second mix monomer lotion is under normal temperature conditions glassy state at 50 degree or so, has certain toughness;
In the core-shell structure of the second mix monomer lotion, the particle in the second mix monomer lotion is wrapped in conduct as the first shell
The nanometer silicon dioxide particle of core.
When preparing third mix monomer lotion in the method for the present invention, styrene, methyl methacrylate, acrylic acid have been used
And butyl acrylate, according to the copolymer that the component proportion of the method for the present invention obtains, i.e. third mix monomer lotion, according to copolymerization
The glass transition temperature formula of object calculates it is found that since there are cross-linked structure, third mixing in third mix monomer emulsion system
The glass transition temperature of monomer emulsions improves the intensity of latex particle shell at 80 degree or so, makes finally obtained composite fire-proof
The fire-resistant fluid of glass becomes a kind of structure of hard outside soft inside, i.e., in the fireproof gum for guaranteeing that the fire-resistant fluid of composite fireproof glass is solidified into
Under conditions of higher-strength, still there is certain toughness.In the core-shell structure of third mix monomer lotion, third mixing
The particle of monomer emulsions is wrapped in the particle of the second mix monomer lotion as the first shell as the second shell.
The fire-resistant fluid of the composite fireproof glass of the method for the present invention preparation, using the method for preparing core-shell emulsion, core
It is the mixture based on silica, it is hydroxide outside two layers of colloid shell that two layers of colloid shell has been wrapped up in outside
Potassium solution, two layers of colloid sheath polymers can absorb ultraviolet light, extend the service life of composite fireproof glass, it is often more important that one
The colloid shell for determining thickness can keep apart silica dioxide granule and potassium hydroxide solution at normal temperature or low temperature, in room temperature or
When low temperature, silica dioxide granule and potassium hydroxide solution can not be contacted, and not reacted, and when temperature is higher, i.e., higher than colloid
When the glass transition temperature of shell, colloid shell becomes rubbery state from glassy state, and potassium hydroxide solution penetrates into colloid shell, with two
Silicon oxide particle reacts to obtain potassium silicate solution to get to water content very little, and modulus is the potassium water glass of 4-6, and is added
Prodan, can accelerate the curing rate of potassium water glass, improve the intensity after potassium water glass solidifies;Shape after potassium water glass hardening
At silica network skeleton, at high temperature hardness decline very little, have good anti-flammability, can high temperature resistant can prevent fires, firmly
Degree is higher, enhances the hardness and heat resistance of composite fireproof glass;Simultaneously because containing acrylic acid and methacrylic acid in colloid,
Acrylic acid and methacrylic acid all have hydrophily, contain some water in colloid, and when meeting fire, water will ooze out, and also rise and centainly go out
Fire action;The fire-resistant fluid for the composite fireproof glass that the method for the present invention is prepared using core-shell structure, by the low neat soap shell of 70%-75%
Lotion and potassium hydroxide solution are mixed, and generate potassium silicate at a certain temperature, and water content is few, and modulus is high, and (modulus refers to
The molecular proportion or molar ratio of silica and alkali metal oxide in waterglass), it can play bigger effect in fire prevention, while because
Water content is few, and fireproof gum made of the fire-resistant fluid solidification of above-mentioned composite fireproof glass substantially increases composite fire-proof glass without microvesicle
The apparent property and fireproofing and heat resistant of glass.
On the other hand, the present invention provides a kind of fire-resistant fluids of composite fireproof glass;The fire prevention of above-mentioned composite fireproof glass
Liquid is prepared by above-mentioned preparation method.
Embodiment 8
As shown in Figure 1, the present invention is prepared for a kind of composite fireproof glass, it is made of the first glass 1 and the second glass 21, the
One glass 1 and the second glass 21 are laminated together by the cohesiveness for glue-line 3 of preventing fires, and fire prevention glue-line 3 is prepared by embodiment 1
The fire-resistant fluid of composite fireproof glass solidifies, fire prevention glue-line 3 with a thickness of 1mm.
Embodiment 9
As shown in Fig. 2, the present invention is prepared for a kind of composite fireproof glass, by the first glass 1, the second glass 21, third glass
Glass 22, the 4th glass 23 and the 5th glass 24 composition, above-mentioned 5 sheet glass are laminated together by the cohesiveness for glue-line 3 of preventing fires, on
It states the fire-resistant fluid that fire prevention glue-line 3 is the composite fireproof glass prepared by embodiment 1 to solidify, the thickness of above-mentioned fire prevention glue-line 3
For 2mm.
As the preferred of above-described embodiment, the outer surface of the second glass 21 can by the laminated divided glass of glue-line 3 of preventing fires,
For example, the second glass 21 is laminated by the cohesiveness and third glass 22 of fire prevention glue-line 3, third glass 22 passes through fire prevention glue-line 3
Laminated with the 4th glass 23, the 4th glass 23 is laminated by fire prevention glue-line 3 and the 5th glass 24, and the 5th glass 24 passes through fireproof gum
Layer 3 and the 6th glass are laminated etc..
Apply the preferred of example as above-mentioned, above-mentioned fire prevention glue-line 3 with a thickness of 1mm-2mm, the first glass 1, the second glass 21,
The thickness of third glass 22, the 4th glass 23 and the 5th glass 24 is 4mm.
The method for preparing above-mentioned composite fireproof glass are as follows:
A, prepare the glass of 5 4mm thickness, wherein 4 are chemically toughened glass, 1 is non-chemical tempered glass;
B, by the fire-resistant fluid of the above-mentioned composite fireproof glass prepared, above-mentioned 4 chemistry are overlying on by sheet form of drying in the air respectively
Tempered glass surface, and be 80 DEG C in temperature, humidity 60%, under conditions of the system of drying in the air 12 hours, obtain with thick anti-of 1.5mm
4 chemically toughened glass of fiery glue-line;Wherein, temperature processed of drying in the air can be 75 DEG C -85 DEG C, and humidity can be 50%-70%, fire prevention
The thickness of glue-line can be 1-2mm;Above-mentioned 4 chemically toughened glass are labeled as the second glass glass, third glass, the 4th glass
Remaining 1 non-chemical tempered glass is labeled as the first glass by glass and the 5th glass;
C, by the 4th glass without fire prevention glue-line a face gland the 5th glass tape fire prevention glue-line one side on, two pieces of glass
Glass is adhered to each other by the intermediate stickiness for preventing fires glue-line;
D, with method identical with step c successively by third glass without fire prevention glue-line a face gland in the 4th glass tape
Prevent fires glue-line one side on, by the second glass without fire prevention glue-line a face gland third glass tape fire prevention glue-line one side
On;
E, by the first glass gland in the one side of the second glass tape fire prevention glue-line, as shown in Figure 2;
F, above-mentioned laminated good composite fire-proof glass is put into still kettle and is forced into 0.5Mpa, pressurize while being warming up to 80 DEG C
Left and right and steam pressure 30min, after being cooled to room temperature take out to get to tool be of five storeys 4 layers of glass prevent fires glue-lines composite fireproof glass;
Wherein, above-mentioned fire prevention glue-line is solidified by the fire-resistant fluid of above-mentioned composite fireproof glass.
The method that the fire-resistant fluid of composite fireproof glass is prepared using embodiment 1-7 is prepared for the anti-of 7 kinds of composite fireproof glass
Fiery liquid, correspondingly, passing through the above-mentioned method for preparing composite fireproof glass, system using the fire-resistant fluid of above-mentioned 7 kinds of composite fireproof glass
Obtained 7 composite fireproof glass identical with the composite fireproof glass structure of embodiment 9.
Comparative example 1
Fire-resistant fluid using pure potassium water glass as composite fireproof glass passes through the above-mentioned side for preparing composite fireproof glass
Method prepares composite fireproof glass identical with 9 structure of embodiment.
Comparative example 2
1kg water is taken, 1kg modulus is the potassium water glass of 2.9-3.4, is uniformly mixed and forms potassium water glass;Using potassium water glass
It is prepared identical as 9 structure of embodiment as the fire-resistant fluid of composite fireproof glass by the above-mentioned method for preparing composite fireproof glass
Composite fireproof glass.
Fire resistance test experience is carried out to above-mentioned 9 pieces of composite fireproof glass according to GB/T12513-2006 national standard,
The fire prevention time of each composite fireproof glass is obtained, experiment takes parallel sample 4, takes its statistical average as experimental result;
The form observed by the naked eye obtains apparent mass;It is multiple using 7 pieces of the fire-resistant fluid preparation of the composite fireproof glass of embodiment 1-7
See Table 1 for details for the performance parameter for 2 pieces of composite fireproof glass that conjunction flame resistant glass and comparative example 1-2 are provided:
The fire protecting performance parameter list of 1. 9 pieces of composite fireproof glass of table
Embodiment glass |
Transmitance |
Prevent fires time/min |
Apparent mass |
1 glass of embodiment |
79% |
69 |
Without microvesicle |
2 glass of embodiment |
81% |
77 |
Without microvesicle |
3 glass of embodiment |
82% |
79 |
Without microvesicle |
4 glass of embodiment |
84% |
81 |
Without microvesicle |
5 glass of embodiment |
83% |
82 |
Without microvesicle |
6 glass of embodiment |
83% |
81 |
Without microvesicle |
7 glass of embodiment |
85% |
84 |
Without microvesicle |
1 glass of comparative example |
58% |
41 |
There is microvesicle |
2 glass of comparative example |
61% |
49 |
There is microvesicle |
Note: above-mentioned glass refers to the composite fireproof glass of the fire-resistant fluid preparation using the composite fireproof glass of embodiment 1-7.
It is obtained by above-mentioned detection method and test data, is made in comparative example 1 or 2 using potassium water glass or pure potassium water glass
For composite fireproof glass fire-resistant fluid and the composite fireproof glass for preparing, inside there are a large amount of microvesicles, and the time of preventing fires is shorter;
There is microvesicle, the fire prevention time is short, illustrates that water content is more in the fire-resistant fluid of the composite fireproof glass of comparative example 1 and comparative example 2, great Liang Wei
The presence of bubble reduces the hardness and fireproofing and heat resistant performance of composite fireproof glass, and affects the apparent matter of composite fireproof glass
Amount.
By using embodiment 1-7 composite fireproof glass fire-resistant fluid preparation 7 pieces of composite fireproof glass, no microvesicle,
The fire prevention time is longer, and apparent property is good;Without microvesicle, the time of preventing fires is longer, illustrates the anti-of composite fireproof glass of the invention
Water content is few in fiery liquid, and without microvesicle in glue-line of preventing fires, composite fireproof glass has preferable fireproofing and heat resistant performance;Again because above-mentioned multiple
It closes in the fire-resistant fluid of flame resistant glass containing only micro emulsifier, not only makes the fire-resistant fluid dispersion of composite fireproof glass more steady
It is fixed, and also reduce the production cost of the fire-resistant fluid of composite fireproof glass.
Disclosed above is only a specific embodiment of the invention, but scope of protection of the present invention is not limited thereto, is appointed
What those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, answer
It is included within the scope of the present invention.Therefore, protection scope of the present invention should be with above-mentioned scope of protection of the claims
It is quasi-.