CN101817647B - Composite heat-insulating fire-proof glass with high integral adhesion and manufacturing method thereof - Google Patents

Composite heat-insulating fire-proof glass with high integral adhesion and manufacturing method thereof Download PDF

Info

Publication number
CN101817647B
CN101817647B CN 201010169770 CN201010169770A CN101817647B CN 101817647 B CN101817647 B CN 101817647B CN 201010169770 CN201010169770 CN 201010169770 CN 201010169770 A CN201010169770 A CN 201010169770A CN 101817647 B CN101817647 B CN 101817647B
Authority
CN
China
Prior art keywords
glass
fire
composite heat
fused salt
proof
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN 201010169770
Other languages
Chinese (zh)
Other versions
CN101817647A (en
Inventor
宋丽
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hubei Jin Jing Green special glass Co., Ltd.
Shandong Jin Jing Green fireproof glass Co., Ltd.
Original Assignee
宋丽
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 宋丽 filed Critical 宋丽
Priority to CN 201010169770 priority Critical patent/CN101817647B/en
Publication of CN101817647A publication Critical patent/CN101817647A/en
Application granted granted Critical
Publication of CN101817647B publication Critical patent/CN101817647B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Abstract

The invention provides composite heat-insulating fire-proof glass with high integral adhesion, which has a sandwich structure consisting of at least two glass layers and a fire-proof adhesive layer between the two adjacent glass layers, wherein at least one glass layer is made of the glass obtained by chemical treatment; the chemical treatment is carried out by placing flat glass in a molten salt tank of an exchange furnace and then performing ion exchange on the flat glass and the sylvite-containing molten salt in the molten salt tank; and the molten salt also contains one or more alkali metal antimonates. The composite heat-insulating fire-proof glass with high integral adhesion of the invention greatly improves the fire resistance; the adhesion of the foamed fire-proof adhesive layer is also greatly improved; and even if the flushing is performed under a high temperature condition, the integrity of the glass is maintained well, so that the glass has good fire resistance and heat insulation performance in actual fire prevention and fire fighting operation.

Description

Composite heat-insulating fire-proof glass that a kind of integral adhesion is high and method of manufacture thereof
Technical field
The present invention relates to the method for manufacture of the high composite heat-insulating fire-proof glass of a kind of integral adhesion and the new composite heat-insulating fire-proof glass that obtains through this method of manufacture.
Background technology
Flame resistant glass is meant under regulation fire testing condition; The special glass that can keep its integrity and thermal insulation; It can be after fire takes place; Being kept perfectly property, and formation as far as possible for a long time is effectively fire prevention, Smoke prevention, radioprotective barrier together, is the requisite safe building materials of Highrise buildings, communal facility; At present, flame resistant glass mainly contains following several kinds both at home and abroad:
A kind of flame resistant glass is a single-sheet fire-resistant glass, wherein is typically borosilicate single-sheet fire-resistant glass and caesium potassium single-sheet fire-resistant glass:
The remarkable fire resistance of borosilicate single-sheet fire-resistant glass stems from its very low thermal expansivity, is merely 4 * 10 -6(20-300 ℃) is than low 2 to 3 times of simple glass (silicate glass).In addition, the borosilicate single-sheet fire-resistant glass also has high softening-point, outstanding speciality such as fabulous thermal-shock resistance and viscosity.Therefore, when fire took place, the borosilicate single-sheet fire-resistant glass was difficult for expanding cracked, thereby meets the requirements of the fire prevention time limit.
Another kind is that caesium potassium single-sheet fire-resistant glass is to be handled and physical toughened being made through particular chemical by common float glass.Such glass keeps the naked light and poisonous, the obnoxious flavour of fire integrity, blocking-up counter-fire face in the regular hour, but does not possess the adiabatic effect of thermal insulation.Belong to C class flame resistant glass.
Another kind is the heat insulation type flame resistant glass:
When fire took place, the glass that can satisfy fire integrity and thermal insulation within a certain period of time was called the heat insulation type flame resistant glass.Flame can produce high heat in combustion processes, and sees through glass with thermal radiation and heat conducting mode, and the temperature that makes glass carry on the back fiery face constantly raises.When acquiring a certain degree, heat can make people or combustiblematerials under the situation that does not touch flame, is burnt or ignites.The heat insulation type flame resistant glass injures in order to make escape and rescue personnel exempt from heat just, and the destructiveness of fire is reduced to minimum design.Its special fire-retardant material can absorb heat significantly, thereby it is controlled in the standard value, and the most effective safeguard protection is provided.
The heat insulation type flame resistant glass comprises the compound insulating fire-retarding glass and the heat insulation type flame resistant glass etc. that is in the milk.
Compound insulating fire-retarding glass is composited by two-layer or former one deck that attaches of multiple glazing or multi-layer fireproofing plastic clip layer usually.When fire takes place; Side towards the fire glass bursts after meeting high temperature very soon; Fire prevention plastic clip layer is about about ten times of foaming and intumescings in succession, and the high calorie that absorbs flame in a large number and brought, and form the White-opalescent Formica; Its hard degree can guarantee fire integrity, and the porous structure makes it have heat-blocking action.Therefore, compound insulating fire-retarding glass both can intercept high temperature effectively, can completely cut off flame, smog and toxic gas again, can in fire, avoid causing personnel's fear.
Grouting type flame resistant glass is by after the sealing of two sheet glass process, pours into inorganic fire glue therebetween and is made.When fire took place, side towards the fire glass burst after meeting high temperature very soon, and the inorganic fire glue-line scleroma rapidly that central, clear is gelatin forms a White-opalescent fire-proof heat insulation board, and the high calorie that absorbs flame in a large number and brought.When stoping propagation of flame, also stop the high temperature fiery face conduction of supporting or opposing.
Wherein, composite fireproof glass is effectively aspect heat insulation, fire prevention.Now existing a lot of related patent U.S. Patent No. (application) disclose the method for making this composite fireproof glass.
Such as, U.S. Pat 4,190,698 disclose prescription and the method for manufacture that is used for composite fireproof glass.The open WO01/70495 of international application also discloses a kind of method of manufacture of refractory glass.
Summary of the invention
Contriver of the present invention finds, for composite fireproof glass, in order to improve its intensity, reaches excellent resistivity against fire, requires the tackiness between the fire prevention glue after employed glass and the foaming further to improve, and just requires the integral adhesion raising.If above-mentioned tackiness is not enough, possibly cause when catching fire, the fire prevention glue after the glass of carrying on the back fiery face and the foaming breaks away from, thereby the intensity of fire prevention glue is diminished and collapses, and has lost the fp performance.For this technical problem, all do not relate in the existing disclosed document, do not relate to the method how to solve this technical problem yet.
The present invention is directed to the above-mentioned technical problem that will solve, the compound insulating fire-retarding glass of HS that the tackiness of the fire prevention glue after a kind of glass being provided and having foamed significantly improves; A kind of method of manufacture of making this composite heat-insulating fire-proof glass also is provided.
1. composite heat-insulating fire-proof glass that integral adhesion is high, it has the sandwich structure that is made up of the fire prevention glue-line between layer glass and the adjacent two layers glass at least;
Wherein, the said glass of one deck at least is through chemically treated chemical treatment glass, and this chemical treatment is that sheet glass is put into stove of exchanging fused salt groove, carries out with the fused salt that comprises sylvite in the fused salt groove that IX obtains; Said fused salt also contains one or more basic metal stibnates.
2. according to the high composite heat-insulating fire-proof glass of technical scheme 1 described integral adhesion, it is characterized in that the temperature of fused salt remains in 450~470 ℃ the scope in the said stove of exchanging fused salt groove, ion-exchange time is 6~8 hours.
3. according to technical scheme 1 or the high composite heat-insulating fire-proof glass of 2 described integral adhesions, it is characterized in that said sandwich structure obtains through recombination process is compound, this recombination process may further comprise the steps:
I. the processing belt membrance chemistry is handled the step of glass; Be used to form the liquid fire-retardant material compsn of fire prevention glue-line in first cast on glass of horizontal positioned; And drying should liquid state fire-retardant material compsn, obtains a side surface and has prevent fires the uniformly band film glass of glue-line of thickness;
II. composite steps covers above-mentioned band film glass surface with second block of glass, obtains compound glass;
III. compound pressurization steps along pressurizeing perpendicular to the direction on above-mentioned compound glass surface, obtains this composite heat-insulating fire-proof glass;
Said first block of glass and/or second block of glass are said chemical treatment glass.
4. according to the high composite heat-insulating fire-proof glass of technical scheme 3 described integral adhesions, it is characterized in that said recombination process is further comprising the steps of:
After step, said compound glass as first block of glass, is repeated above-mentioned I-II at this II, continues compound one or more layers fire prevention glue-line and glass, all compound good after, carry out III again and go on foot, said one or more layers glass is preferably chemical treatment glass.
5. according to technical scheme 3 or the high composite heat-insulating fire-proof glass of 4 described integral adhesions, it is characterized in that,
Said liquid fire-retardant material compsn comprises hydrated alkali metal silicate, and the concentration of this hydrated alkali metal silicate is preferably 37~40 degree Beaume especially.
6. according to the high composite heat-insulating fire-proof glass of technical scheme 5 described integral adhesions, it is characterized in that the modulus of said hydrated alkali metal silicate is 3.5~3.7.
7. the preparation method of the composite heat-insulating fire-proof glass that an integral adhesion is high, it has the sandwich structure that is made up of the fire prevention glue-line between layer glass and the adjacent two layers glass at least;
Wherein, the said glass of one deck at least is through chemically treated chemical treatment glass, and this chemical treatment is that sheet glass is put into stove of exchanging fused salt groove, carries out with the fused salt that comprises sylvite in the fused salt groove that IX obtains; Said fused salt also contains one or more basic metal stibnates.
8. according to the preparation method of the high composite heat-insulating fire-proof glass of technical scheme 7 described integral adhesions, it is characterized in that the temperature of fused salt remains in 450~470 ℃ the scope in the stove of exchanging fused salt groove, ion-exchange time is 6~8 hours.
9. according to the preparation method of the high composite heat-insulating fire-proof glass of technical scheme 7 or 8 described integral adhesions, it is characterized in that said sandwich structure is through the recombination process compound, this recombination process may further comprise the steps:
I. the processing belt membrance chemistry is handled the step of glass; Be used to form the liquid fire-retardant material compsn of fire prevention glue-line in first cast on glass of horizontal positioned; And drying should liquid state fire-retardant material compsn, obtains a side surface and has prevent fires the uniformly band film glass of glue-line of thickness;
II. composite steps covers above-mentioned band film glass surface with second block of glass, obtains compound glass;
III. compound pressurization steps along pressurizeing perpendicular to the direction on above-mentioned compound glass surface, obtains this composite heat-insulating fire-proof glass;
Said first block of glass and/or second block of glass are said chemical treatment glass.
Preferably, after the step, said compound glass as first block of glass, is repeated above-mentioned I-II at this II, continues compound one or more layers fire prevention glue-line and glass all compound well after, carry out III again and go on foot, said one or more layers glass is preferably chemical treatment glass.
10. according to the high composite heat-insulating fire-proof glass of technical scheme 7~9 each described integral adhesions, it is characterized in that,
Said liquid fire-retardant material compsn comprises hydrated alkali metal silicate, and the concentration of hydrated alkali metal silicate is preferably 37~40 degree Beaume especially, and the modulus of said hydrated alkali metal silicate is 3.5~3.7.
Do not carry out chemically treated glassy phase ratio with use, used with the fused salt that contains stibnate and carried out chemically treated glass, fire performance has significantly raising; Beat all especially is that the tackiness of the fire prevention glue-line after the foaming also has significantly raising, even under the condition of high temperature, wash by water, also can keep the integrity of glass preferably, thereby in reality fire prevention and fire-fighting operation, plays good fire prevention, heat-proof quality.Embodiment
Aforementioned and other characteristics of the present invention will be described more comprehensively and in claim, particularly point out hereinafter; Following specification sheets is set forth example embodiment more of the present invention in detail; But, these embodiments are just represented the several different mode that principle of the present invention can be used.Referring to preferred embodiment following, other advantages of the present invention and characteristic it will be apparent to those skilled in the art that.
For the T.T. that uses among the present invention, those skilled in the art are appreciated that based on general knowledge.
" modulus " is meant the molecule mol ratio of silicon-dioxide and alkalimetal oxide in the hydrated alkali metal silicate.
" liquid fire-retardant material compsn " is meant the raw material that is used to make the fire prevention glue-line (being also referred to as: intumescent material, fire retardant material layer or flame retardant coating) that is sandwiched between two sheet glass.
" sheet glass " is meant the simple glass plate of surface smoothing, can use existing arbitrarily sheet glass, can used thickness be the sodium calcium float glass of 2.0~4.0mm typically.
" band membrance chemistry handle glass " is meant at the glass composite structure that chemical treatment is on glass after being provided with the fire prevention glue-line.
" hydrated sodium silicate " is also referred to as sodium silicate or bubble flower alkali.
According to one embodiment of the present invention, a kind of composite heat-insulating fire-proof glass is provided, it comprises the sandwich structure that sheet glass and fire prevention glue-line constitute, wherein, this sheet glass is through chemically treated sheet glass.Said chemical treatment is with ordinary plate glass, in comprising the fused salt of sylvite, carries out IX like float glass and obtains.Explanation will abbreviate " chemical treatment glass " through chemically treated sheet glass as among the present invention for ease.
In the preferred embodiments of the disclosure, in chemical treating process, selected sheet glass is put into stove of exchanging fused salt groove, the composition of the fused salt in the fused salt groove comprises: main raw is one or more sylvite, preferably contains saltpetre.The content of this sylvite is preferably 96~98 weight % of fused salt.This fused salt also preferably contains additive, and this additive contains from Al 2O 3, B 2O 3, ZrO 2, select in the MOX such as ZnO and/or MgO one or more, its content is preferably 0.5~3 weight % of fused salt, preferred 1~2 weight %; Also contain one or more basic metal stibnates; Content is fused salt 1~2.5 weight %; As: potassium antimonate, potassium pyroantimoniate, potassium metaantimonate, metaantimmonic acid lithium, pyroantimonic acid lithium, metantimonic acid lithium, sodium antimonate, sodium pyroantimoniate, sodium antimoniate, metaantimmonic acid caesium, pyroantimonic acid caesium and/or metantimonic acid caesium, wherein preferred: potassium antimonate, potassium pyroantimoniate and/or potassium metaantimonate.
Glass is when carrying out above-mentioned chemically treated IX; The temperature of fused salt preferably remains in 450~470 ℃ the scope in the stove of exchanging fused salt groove; If temperature is too low, can't fully carry out IX, thus the tackiness of the fire prevention glue after can reducing glass to a certain extent and foaming; If temperature is too high, the tackiness of the fire prevention glue after also can to a certain degree reducing glass and foaming preferably remains on 450~460 ℃.
The ion-exchange time of glass when carrying out chemical treatment; Thickness according to glass is different, and can control its swap time is 6~8 hours, and the time is too short; Can't fully carry out IX, thus the tackiness of the fire prevention glue after can reducing glass to a certain extent and foaming; If the time is oversize, the tackiness of the fire prevention glue after also can to a certain degree reducing glass and foaming is preferably 6~7 hours.
The stress of the glass after chemical treatment of this embodiment is different and different according to thickness of glass, is generally greater than 450MPa.Compare with the simple glass without chemically treated same thickness, intensity improves about ten times, and the glass after this kind method is handled has following advantage:
1) can not produce tangible optical skew,
2) bearing stress is very high, but the interior card stress that balances each other with it is very little, and there is not the self-destruction phenomenon in this glass,
3) still can cut through the glass after the chemical treatment.
Through the sheet glass and the sandwich structure that the fire prevention glue-line constitutes of above-mentioned chemical treatment, can make through the complex method of routine, thereby obtain composite heat-insulating fire-proof glass of the present invention.For the intensity of further chemical treatment composite heat-insulating fire-proof glass, preferred complex method may further comprise the steps:
I. the processing belt membrance chemistry is handled the step of glass; Be used to form the liquid fire-retardant material compsn of fire prevention glue in first chemical treatment cast on glass of horizontal positioned; And drying should liquid state fire-retardant material compsn, obtains a side surface and has prevent fires the uniformly band membrance chemistry of glue-line of thickness and handle glass;
II. composite steps covers above-mentioned band membrance chemistry with second glass and handles glass surface, obtains compound glass; This second glass can be without chemically treated simple glass, perhaps preferably also is chemical treatment glass;
III. compound pressurization steps along pressurizeing perpendicular to the direction on above-mentioned compound glass surface, obtains this composite heat-insulating fire-proof glass.
In the above-mentioned I step of embodiment of the present invention, said liquid fire-retardant material compsn can be existing any liquid fire-retardant material compsn that composite fireproof glass of the same type uses that is used for making.
In order further to strengthen the clinging power between fire prevention glue and the chemical treatment glass, preferred said liquid fire-retardant material compsn comprises hydrated alkali metal silicate, and the concentration of hydrated alkali metal silicate especially preferably is controlled at the 37-40 degree Beaume.With the hydrated alkali metal silicate in this concentration range, tackiness further improves between prepared fire prevention glue-line and the above-mentioned chemical treatment glass, and prevents fires glue-line after foaming, and tackiness also further improves between the above-mentioned chemical treatment glass.
This hydrated alkali metal silicate is preferably the mixture of hydrated sodium silicate, silicate hydrate potassium or hydrated sodium silicate and silicate hydrate potassium; Particularly preferably be hydrated sodium silicate, perhaps the mixture of hydrated sodium silicate and silicate hydrate potassium; Hydrated sodium silicate most preferably.
The hydrate that this hydrated alkali metal silicate is alkalimetal silicate (that is: water glass or bubble flower alkali), its modulus, that is: the molecule mol ratio of silicon-dioxide and alkalimetal oxide is preferably 3.5-3.7.This modulus scope helps that tackiness further improves between prepared fire prevention glue-line and the above-mentioned chemical treatment glass.And the resistivity against fire of fire prevention glue is better.
In addition; Above-mentioned liquid fire-retardant material compsn can also contain other known useful additives; Such as fire retardant, stablizer, char-forming agent, softening agent etc., those skilled in the art can select according to general knowledge, only otherwise the performance that influences composite heat-insulating fire-proof glass of the present invention gets final product.
As the preferred embodiment of the present invention; Consider from the heat-insulating, fire-preventing aspect of performance; Should the liquid state flame-retardant material composite be following composition preferably: said liquid flame-retardant material composite comprises in weight part: base-material: 100 parts, this base-material is above-mentioned hydrated alkali metal silicate softening agent: 5-12 part; Char-forming agent: 1.0-2.5 part; Stablizer: 0.1-10 part; Skimmer: 0-0.05 part; Fire retardant: 0.1-0.3 part.
Said char-forming agent is sugar preferably, one or more that further preferably from the group of being made up of white sugar, glucose, seminose, semi-lactosi, select.With respect to 100 weight part base-materials, the weight part of this char-forming agent is 1.0-2.5.
One or more that said stablizer (also claiming flame retardant) is preferably selected from the group of being made up of urea, trimeric cyanamide, tripoly phosphate sodium STPP, ammonium polyphosphate, Z 150PH, polyoxyethylene glycol, (methyl) vinylformic acid, (methyl) propenoate.With respect to 100 weight part base-materials, the weight part of this stablizer is 0.1-10.
One or more that said fire retardant is preferably selected from the group of being made up of boric acid, borax, with respect to 100 weight part base-materials, the weight part of this fire retardant is 0.1-0.3.
Said skimmer can use conventional skimmer, and for example: tributyl phosphate etc., with respect to 100 weight part base-materials, the weight part of this skimmer is 0-0.05 part.
Said softening agent is preferably 5~12 weight parts.Said softening agent is polyol preferably.Further preferably, this polyol is from by glycerine, terepthaloyl moietie, 1, one or more that select in the group that 2-Ucar 35, tetramethylolmethane, NSC 6366, Xylitol, sorbyl alcohol are formed.
Before the I step, in order to form the uniform liquid level of thickness, also preferably include the sticking limit of chemical treatment glass step, this step is to prevent the leakproof bar that liquid fire-retardant material combination of compositions thing spills at the chemical treatment glass surface along the periphery adhesion.
Cast is preferred slowly cast, prevents that the fire-retardant material liquid composite from spilling, and after leaving standstill, this liquid level becomes level, forms the uniform liquid level of thickness, and the thickness of this liquid level is preferably 3.5-5mm.Dry 12-72 hour, obtain a side surface and have prevent fires the uniformly band membrance chemistry of glue-line of thickness and handle glass
Between I and II step, will be with membrance chemistry to handle glass cutting is specified dimension, if used the leakproof bar, need cut leakproof bar part, obtains handling glass by the band membrance chemistry that fire prevention glue-line and chemical treatment glass constitute.
If desired; In the II step; Can further handle glass at compound one or more layers band membrance chemistry of the chemical treatment glass side continuation of this compound glass, wherein, the fire retardant face that this one or more layers band membrance chemistry is handled glass carries out compound to this compound glass.This recombination process and said process are similar, do not have other special requirements.
III. compound pressurization steps along pressurizeing perpendicular to the direction on above-mentioned compound glass surface, obtains this composite heat-insulating fire-proof glass.
The pressure of pressurization can come as required to confirm that be preferably 0.5-1.2Mpa, the time is 1.5-4 hour.
Composite heat-insulating fire-proof glass of the present invention is owing to adopted the chemical treatment glass of chemical treatment; So the intensity and the fire resistance of glass itself are improved on the one hand; More beat all is this chemical treatment glass and the tackiness of fire prevention glue-line has had large increase; Particularly after the fire prevention glue-line is met the fire foaming, it is on glass to adhere to chemical treatment securely, in fire, can guarantee the integrity and the thermal insulation of flame resistant glass well.
Making us more beyond thought is; According to composite heat-insulating fire-proof glass of the present invention, after detecting its fire insulation performance, dash with high pressure water with fire-fighting from back-fire side immediately; The fire prevention glue of glass and foaming can not break away from yet; Can keep its integrity, thereby prove that this composite heat-insulating fire-proof glass has excellent intensity, can guarantee the integrity and the thermal insulation of flame resistant glass well in fire.
This compound back insulating fire-retarding glass handling ease because glass is high with tackiness between the fire prevention glue-line, is not separated so when cutting, can not make between glass and the fire prevention glue-line yet, can not make the glass fragmentation yet.
Below through concrete embodiment technical scheme of the present invention and effect thereof are further specified.
< preparation example >
Preparation example 1
(1) preparation chemical treatment glass
The preparation fused salt, with KNO 3Powder is at fused salt groove internal heating to 450 ℃, and fusing fully adds additive, and additive is potassium pyroantimoniate and Al 2O 3Mixture, stir and to make additive and saltpetre thorough mixing, behind the adding additive, with respect to the total amount KNO of fused salt 3Account for 97 weight %, Al 2O 3Account for 1 weight %, potassium pyroantimoniate accounts for 2 weight %, generates as clear as crystal fused salt, and the contamination precipitation in the fused salt is in bottom land.
Chemical treatment, select high-quality original sheet glass, thick 3mm, 2100mm * 650mm carries out the circular arc polishing to its periphery, and temperature in the fused salt groove is remained on 460 ℃, subsequently glass is immersed in the above-mentioned fused salt groove, and be 6 hours swap time.Cooling obtains chemical treatment glass then.The stress of this chemical treatment glass is 465MPa.
(2) preparation composite heat-insulating fire-proof glass
Provide prescription liquid fire-retardant material compsn as described in Table 1.
Each component is mixed, stir, obtain liquid fire-retardant material compsn; With obtaining chemical treatment glass in (1), lie on the smooth stand, after the clean; Water around the glass with bonded adhesives and to spill; Again steel tubing in different shapes is adhered to Jiao Mianshang after 15 minutes, the inspection seam crossing guarantees that the seam crossing sealing is tight.
Prepare liquid fire-retardant material compsn, in the hydrated sodium silicate (modulus is 3.5) of 100 weight parts, add softening agent glycerine: 8 parts; Char-forming agent white sugar: 2.0 parts; Stablizer ammonium polyphosphate: 3 parts; Skimmer tributyl phosphate: 0.03 part; The fire retardant borax: 0.3 part, fully stir, obtain the liquid fire-retardant material compsn of homogeneous, the concentration of said hydrated sodium silicate is 38 degree Beaume.
Glass behind the sticking limit is placed the dry stand of level, and horizontal positioned is poured into the above-mentioned liquid fire-retardant material compsn for preparing on glassly lentamente, makes the thick about 4mm of liquid fire prevention glue-line.With this glass standing and drying 24 hours, dried fire prevention bondline thickness was about 1.6mm subsequently, obtained being with membrance chemistry to handle glass.Observe the glue-line surface and inner that should prevent fires, pore-free, inclusion-free, surperficial flawless, thickness is even, smooth, smooth.
Above-mentioned band membrance chemistry is handled glass to be cut; Cut the steel tubing in different shapes part; It is positioned on the platform, and again that another sheet size is identical chemical treatment glass surface covers this band membrance chemistry to fire prevention glue-line, four limits of band membrance chemistry processing glass with aliging and handles on glass.According to upper type, continue to continue compound each 3 layers of identical fire prevention glue-line and chemical treatment glass in the chemical treatment glass side of this compound glass,
Top compound good compound glass is put into autoclave, and constant pressure is 1.2Mpa, and the time is 2 hours, makes the composite heat-insulating fire-proof glass of thick about 23mm of 4 layers of fire prevention of 5 layers of glass glue.
Make 2 such composite heat-insulating fire-proof glass simultaneously.
Preparation example 2
Other conditions are identical with preparation example 1, just the chemical treatment in (1) step changed into:
Chemical treatment, temperature in the fused salt groove is remained on 450 ℃, subsequently glass to be immersed in the above-mentioned fused salt groove, be 6 hours swap time.And potassium pyroantimoniate is replaced with potassium antimonate.
Preparation example 3
Other conditions are identical with preparation example 1, just the chemical treatment in (1) step changed into:
Chemical treatment, temperature in the fused salt groove is remained on 470 ℃, subsequently glass to be immersed in the above-mentioned fused salt groove, be 6 hours swap time.
Preparation example 4
Other conditions are identical with preparation example 1, just the chemical treatment in (1) step changed into:
Chemical treatment, temperature in the fused salt groove is remained on 460 ℃, subsequently glass to be immersed in the above-mentioned fused salt groove, be 8 hours swap time.
Preparation example 5
Other conditions are identical with preparation example 1, just the chemical treatment in (1) step changed into:
Chemical treatment, temperature in the fused salt groove is remained on 440 ℃, subsequently glass to be immersed in the above-mentioned fused salt groove, be 6 hours swap time.
Preparation example 6
Other conditions are identical with preparation example 1, just the chemical treatment in (1) step changed into:
Chemical treatment, temperature in the fused salt groove is remained on 480 ℃, subsequently glass to be immersed in the above-mentioned fused salt groove, be 6 hours swap time.
Preparation example 7
Other conditions are identical with preparation example 1, just the chemical treatment in (1) step changed into:
Chemical treatment, temperature in the fused salt groove is remained on 460 ℃, subsequently glass to be immersed in the above-mentioned fused salt groove, be 12 hours swap time.
Preparation example 8
Other conditions are identical with preparation example 1, just the modulus of the hydrated sodium silicate in (2) step changed into 3.7.
Preparation example 9
Other conditions are identical with preparation example 1, just the modulus of the hydrated sodium silicate in (2) step changed into 3.6.
Preparation example 10
Other conditions are identical with preparation example 1, and just the concentration with the hydrated sodium silicate in (2) step changes 40 degree Beaume.
Preparation example 11
Other conditions are identical with preparation example 1, and just the concentration with the hydrated sodium silicate in (2) step changes 37 degree Beaume.
Preparation example 12
Other conditions are identical with preparation example 1, just the modulus of the hydrated sodium silicate in (2) step changed into 3.0.
Preparation example 13
Other conditions are identical with preparation example 1, just the modulus of the hydrated sodium silicate in (2) step changed into 2.8.
Preparation example 14
Other conditions are identical with preparation example 1, and just the concentration with the hydrated sodium silicate in (2) step changes 30 degree Beaume.
Preparation example 15
Other conditions are identical with preparation example 1, and just the concentration with the hydrated sodium silicate in (2) step changes 25 degree Beaume.
Preparation example 16 (comparative examples)
Other conditions are identical with preparation example 1, just glass do not carried out chemical treatment, directly use original sheet glass to prepare composite heat-insulating fire-proof glass.
Preparation example 17 (comparative examples)
Other conditions are identical with preparation example 1, in (1) step, replace potassium pyroantimoniate with potassium pyrophosphate.
More than the preparation condition of each embodiment and comparative example be documented in the table 1.
The preparation condition of each embodiment of table 1 and comparative example
Component Temperature in the fused salt groove (℃) Swap time (hour) Silicate hydrate na concn (degree Beaume) The hydrated sodium silicate modulus
Preparation example 1 460 6 38 3.5
Preparation example 2 450 6 38 3.5
Preparation example 3 470 6 38 3.5
Preparation example 4 460 8 38 3.5
Preparation example 5 440 6 38 3.5
Preparation example 6 480 6 38 3.5
Preparation example 7 460 12 38 3.5
Preparation example 8 460 6 38 3.7
Preparation example 9 460 6 38 3.6
Preparation example 10 460 6 40 3.5
Preparation example 11 460 6 37 3.5
Preparation example 12 460 6 38 3.0
Preparation example 13 460 6 38 2.8
Preparation example 14 460 6 30 3.5
Preparation example 15 460 6 25 3.5
Preparation example 16 - - 38 3.5
Preparation example 17 460 6 38 3.5
< effect example >
With the composite heat-insulating fire-proof glass that above-mentioned preparation example makes, carry out the experiment of heat-resisting integrity, above-mentioned composite heat-insulating fire-proof glass is installed on the installation window as the test wall of test furnace one sidewall, this test wall can move left and right, separates with test furnace.Heat up according to the international standard heating curve in the stove; Temperature-rise period carries out according to following program: be warmed up to 824 ℃ through 30 minutes; Be warmed up to 945 ℃ through 30 minutes again; Continue test if desired, the climbing speed of temperature can be according to carrying out through the speed that can reach 1006 ℃ in 30 minutes again.With a heating in two composite heat-insulating fire-proof glass in same preparation example or the comparative example; Fire prevention glue foaming and intumescing; Medial temperature up to glass outer surface (carrying on the back fiery face) reaches 140 ℃; Record is the time of heating altogether, explains that this composite heat-insulating fire-proof glass has not had heat-proof quality in this time; The heating of another piece stopped the heating in the test furnace after 60 minutes, in 5 minutes, will test wall and move away test furnace, washed by water 1 minute with directly the support or oppose glass of fiery face of fire-fighting lance, and whether sight glass bursts, comes unstuck.After the bath, the glass number of plies that sight glass is burnt in combustion testing and fire prevention glue-line number.Test result is as shown in table 2
Table 2 test result
Component The stress of chemical treatment glass (MPa) The medial temperature of glass outer surface reach 140 ℃ time (minute) After the bath, the situation of glass The glass number of plies that glass is burnt in combustion testing The fire prevention glue-line number that glass is burnt in combustion testing
Preparation example 1 465 71 1 1
Preparation example 2 473 73 1 1
Preparation example 3 450 70 1 1
Preparation example 4 465 71 1 1
Preparation example 5 380 64 3 2
Preparation example 6 400 66 3 2
Preparation example 7 400 65 3 2
Preparation example 8 465 75 1 1
Preparation example 9 465 73 1 1
Preparation example 10 465 71 1 1
Preparation example 11 465 71 1 1
Preparation example 12 465 63 2 2
Preparation example 13 465 62 2 2
Preparation example 14 465 65 2 2
Preparation example 15 465 64 2 2
Preparation example 16 45 60 × 4 3
Preparation example 17 220 62 × 4 3
In the table: after the ◎ bath, glass does not have and bursts, do not come unstuck, and is kept perfectly;
After zero bath, glass outer bursts, and breaks away from adjacent fire prevention glue, and glass outer collapses and, but inner layer glass also is kept perfectly;
After * the bath, glass outer bursts, and breaks away from adjacent fire prevention glue, and water dashes and passes through glass, and glass can not be kept perfectly
Can know that by above result with the glassy phase ratio that use is not carried out chemically treated glass or handled with phosphatic fused salt, used with the fused salt that contains stibnate and carried out chemically treated glass, fire performance has significantly raising; And the tackiness of the fire prevention glue-line after the foaming also improves a lot, even under the condition of high temperature, wash by water, also can keep the integrity of glass preferably, thereby in reality fire prevention and fire-fighting operation, plays good fire prevention, heat-proof quality.
Particularly preferably be, when glass was carried out chemical treatment, the temperature of fused salt preferably remained in 450~470 ℃ the scope in the stove of exchanging fused salt groove; The preferred time of IX was controlled at 6~8 hours; The silicate hydrate na concn that is used for making the liquid flame-retardant material composite of fire prevention glue is preferably the 37-40 degree Beaume, and the hydrated sodium silicate modulus is preferably 3.5~3.7, under such optimum condition; Even under the condition of high temperature, wash by water; Can not make back of the body flint glass burst, come unstuck yet, thus can keep the integrity of glass well, thus in reality fire prevention and fire-fighting operation, can play extraordinary fire prevention, heat-proof quality.Such excellent properties is very valuable in actual use.
Those skilled in the art can carry out about various improvement of the present invention and variation under the guidance of above instruction.Therefore, it is understandable that, under the situation of the invention thinking that does not break away from claim of the present invention, can be with other mode embodiment of the present invention except the specifically described mode of this paper.

Claims (15)

1. composite heat-insulating fire-proof glass that integral adhesion is high, it has the sandwich structure that is made up of the fire prevention glue-line between layer glass and the adjacent two layers glass at least;
Wherein, the said glass of one deck at least is through chemically treated chemical treatment glass, and this chemical treatment is that sheet glass is put into stove of exchanging fused salt groove, carries out with the fused salt that comprises sylvite in the fused salt groove that IX obtains; Said fused salt also contains one or more basic metal stibnates.
2. the high composite heat-insulating fire-proof glass of integral adhesion according to claim 1; It is characterized in that; The temperature of fused salt remains in 450~470 ℃ the scope in the said stove of exchanging fused salt groove; Ion-exchange time is 6~8 hours, and the content of said one or more basic metal stibnates is 1~2.5 weight % of fused salt.
3. the high composite heat-insulating fire-proof glass of integral adhesion according to claim 1 and 2 is characterized in that said sandwich structure obtains through recombination process is compound, and this recombination process may further comprise the steps:
I. the processing belt membrance chemistry is handled the step of glass; Be used to form the liquid fire-retardant material compsn of fire prevention glue-line in first cast on glass of horizontal positioned; And drying should liquid state fire-retardant material compsn, obtains a side surface and has prevent fires the uniformly band film glass of glue-line of thickness;
II. composite steps covers above-mentioned band film glass surface with second block of glass, obtains compound glass;
III. compound pressurization steps along pressurizeing perpendicular to the direction on above-mentioned compound glass surface, obtains this composite heat-insulating fire-proof glass;
Said first block of glass and/or second block of glass are said chemical treatment glass.
4. the high composite heat-insulating fire-proof glass of integral adhesion according to claim 3 is characterized in that said recombination process is further comprising the steps of:
After step, said compound glass as first block of glass, is repeated above-mentioned I-II at this II, continues compound one or more layers fire prevention glue-line and glass, all compound good after, carry out III again and go on foot.
5. the high composite heat-insulating fire-proof glass of integral adhesion according to claim 4 is characterized in that said one or more layers glass is chemical treatment glass.
6. according to claim 3 or the high composite heat-insulating fire-proof glass of 4 described integral adhesions, it is characterized in that,
Said liquid fire-retardant material compsn comprises hydrated alkali metal silicate.
7. the high composite heat-insulating fire-proof glass of integral adhesion according to claim 6 is characterized in that the concentration of this hydrated alkali metal silicate is 37~40 degree Beaume.
8. the high composite heat-insulating fire-proof glass of integral adhesion according to claim 6 is characterized in that the modulus of said hydrated alkali metal silicate is 3.5~3.7.
9. the method for manufacture of the composite heat-insulating fire-proof glass that an integral adhesion is high, it has the sandwich structure that is made up of the fire prevention glue-line between layer glass and the adjacent two layers glass at least;
Wherein, the said glass of one deck at least is through chemically treated chemical treatment glass, and this chemical treatment is that sheet glass is put into stove of exchanging fused salt groove, carries out with the fused salt that comprises sylvite in the fused salt groove that IX obtains; Said fused salt also contains one or more basic metal stibnates.
10. the method for manufacture of the composite heat-insulating fire-proof glass that integral adhesion according to claim 9 is high; It is characterized in that; The temperature of fused salt remains in 450~470 ℃ the scope in the stove of exchanging fused salt groove; Ion-exchange time is 6~8 hours, and the content of said one or more basic metal stibnates is 1~2.5 weight % of fused salt.
11. the method for manufacture according to the high composite heat-insulating fire-proof glass of claim 9 or 10 described integral adhesions is characterized in that said sandwich structure is through the recombination process compound, this recombination process may further comprise the steps:
I. the processing belt membrance chemistry is handled the step of glass; Be used to form the liquid fire-retardant material compsn of fire prevention glue-line in first cast on glass of horizontal positioned; And drying should liquid state fire-retardant material compsn, obtains a side surface and has prevent fires the uniformly band film glass of glue-line of thickness;
II. composite steps covers above-mentioned band film glass surface with second block of glass, obtains compound glass;
III. compound pressurization steps along pressurizeing perpendicular to the direction on above-mentioned compound glass surface, obtains this composite heat-insulating fire-proof glass;
Said first block of glass and/or second block of glass are said chemical treatment glass.
12. the method for manufacture of the composite heat-insulating fire-proof glass that integral adhesion according to claim 11 is high; It is characterized in that; After step, said compound glass as first block of glass, is repeated above-mentioned I-II at this II; After continuing whole compound the getting well of compound one or more layers fire prevention glue-line and glass, carry out the III step again.
13. the method for manufacture of the composite heat-insulating fire-proof glass that integral adhesion according to claim 12 is high is characterized in that, said one or more layers glass is chemical treatment glass.
14. the method for manufacture of the composite heat-insulating fire-proof glass that integral adhesion according to claim 11 is high is characterized in that,
Said liquid fire-retardant material compsn comprises hydrated alkali metal silicate, and the modulus of said hydrated alkali metal silicate is 3.5~3.7.
15. the method for manufacture of the composite heat-insulating fire-proof glass that integral adhesion according to claim 14 is high is characterized in that, the concentration of said hydrated alkali metal silicate is 37~40 degree Beaume.
CN 201010169770 2010-05-12 2010-05-12 Composite heat-insulating fire-proof glass with high integral adhesion and manufacturing method thereof Expired - Fee Related CN101817647B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 201010169770 CN101817647B (en) 2010-05-12 2010-05-12 Composite heat-insulating fire-proof glass with high integral adhesion and manufacturing method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 201010169770 CN101817647B (en) 2010-05-12 2010-05-12 Composite heat-insulating fire-proof glass with high integral adhesion and manufacturing method thereof

Publications (2)

Publication Number Publication Date
CN101817647A CN101817647A (en) 2010-09-01
CN101817647B true CN101817647B (en) 2012-12-12

Family

ID=42652949

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 201010169770 Expired - Fee Related CN101817647B (en) 2010-05-12 2010-05-12 Composite heat-insulating fire-proof glass with high integral adhesion and manufacturing method thereof

Country Status (1)

Country Link
CN (1) CN101817647B (en)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103317783B (en) * 2013-07-03 2015-07-08 中国建筑材料科学研究总院 Composite fire-resistant glass combination liquid and preparation method thereof as well as composite fire-resistant glass
CN103359957B (en) * 2013-07-03 2015-05-20 中国建筑材料科学研究总院 Composite fire-retardant glass laminating solution, preparation method thereof and composite fire-retardant glass
CN104259049B (en) * 2014-09-01 2017-04-05 浙江鼎昇新材料科技股份有限公司 A kind of painting method and equipment of cleavable composite fireproof glass surface glued membrane
CN113772964B (en) * 2021-09-22 2023-08-01 万津实业(赤壁)有限公司 Glass tempering method

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1212993C (en) * 1998-03-17 2005-08-03 日本板硝子株式会社 Double-glazing unit
CN101219854A (en) * 2007-01-08 2008-07-16 宋丽 Process for manufacturing single-slice fireproof glass and the single-slice fireproof glass
CN101573229A (en) * 2006-10-31 2009-11-04 皮尔金顿集团有限公司 Method for the production of fire ressistant glazings

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1212993C (en) * 1998-03-17 2005-08-03 日本板硝子株式会社 Double-glazing unit
CN101573229A (en) * 2006-10-31 2009-11-04 皮尔金顿集团有限公司 Method for the production of fire ressistant glazings
CN101219854A (en) * 2007-01-08 2008-07-16 宋丽 Process for manufacturing single-slice fireproof glass and the single-slice fireproof glass

Also Published As

Publication number Publication date
CN101817647A (en) 2010-09-01

Similar Documents

Publication Publication Date Title
CN101817647B (en) Composite heat-insulating fire-proof glass with high integral adhesion and manufacturing method thereof
US20050250639A1 (en) Lithium-aluminosilicate flat float glass
US8206620B1 (en) Optically clear fire resistant windows
NO134615B (en)
JPH0769669A (en) Fire prevention safe plate glass
JPH08210041A (en) Fireproof glazing unit
JP4266514B2 (en) Transparent heat-swellable material
CN107090248A (en) A kind of uncured rubber asphalt waterproof coating of flame retardant type and preparation method thereof
DK154444B (en) FIRE RESISTANT RUDE
KR100873652B1 (en) Coating material for retarding flame, manufacturing method of the same, and flame-retarding method of expanded polystyrene particle using the same
KR102200831B1 (en) Quaci-noncombustible heat insulator and manufacturing method of the same
KR20170037417A (en) reinforcing composition for fire-extinguishing , manufacturing method
NO158930B (en) FIRE PROTECTIVE GLASS PANEL.
CN203888302U (en) Spark-impenetrable radiant heat resisting fireproof glass
KR101212022B1 (en) Environment-friendly neutral liquid extinguishing agent composite and manufacturing process of the same
JP2588684B2 (en) Fire-resistant laminated glass structure and method for producing the same
KR100614233B1 (en) Fire protection glass
KR102175376B1 (en) Quaci-noncombustible heat insulator and manufacturing method of the same
CN101544490B (en) Inorganic fireproof coating of indoor ultrathin steel structure
CN108503232A (en) A method of preparing flame resistant glass
JP2005538015A (en) A clear and stable aqueous solution based on water glass for the production of flame resistant glazing
CN108675651A (en) A kind of fire retardant composition and preparation method thereof being used to prepare flame resistant glass
CN107605371A (en) A kind of fire resistant doorsets of resistance to bubble
CN107417080A (en) A kind of preparation method of individual layer fire prevention safety glass
CN102249562A (en) Double-glass non-thermal insulating fireproof glass and manufacturing method

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
EE01 Entry into force of recordation of patent licensing contract

Application publication date: 20100901

Assignee: Beijing Gelin Jingfeng Fireproof Glass Co.,Ltd.

Assignor: Song Li

Contract record no.: 2013990000310

Denomination of invention: Composite heat-insulating fire-proof glass with high integral adhesion and manufacturing method thereof

Granted publication date: 20121212

License type: Exclusive License

Record date: 20130608

LICC Enforcement, change and cancellation of record of contracts on the licence for exploitation of a patent or utility model
EC01 Cancellation of recordation of patent licensing contract

Assignee: Beijing Gelin Jingfeng Fireproof Glass Co.,Ltd.

Assignor: Song Li

Contract record no.: 2013990000310

Date of cancellation: 20150115

LICC Enforcement, change and cancellation of record of contracts on the licence for exploitation of a patent or utility model
ASS Succession or assignment of patent right

Owner name: BEIJING GELIN JINGFENG FIREPROOF GLASS CO.,LTD.

Free format text: FORMER OWNER: SONG LI

Effective date: 20150623

C41 Transfer of patent application or patent right or utility model
TR01 Transfer of patent right

Effective date of registration: 20150623

Address after: 100074 Beijing city Fengtai District Changxindian Daxinzhuang 400

Patentee after: Beijing Gelin Jingfeng Fireproof Glass Co.,Ltd.

Address before: 100074 Beijing city Fengtai District Changxindian Daxinzhuang Industrial Park No. 400

Patentee before: Song Li

TR01 Transfer of patent right
TR01 Transfer of patent right

Effective date of registration: 20180428

Address after: 255000 Shandong Zibo high tech Zone Expressway north of Zhang Bei Road East

Co-patentee after: Hubei Jin Jing Green special glass Co., Ltd.

Patentee after: Shandong Jin Jing Green fireproof glass Co., Ltd.

Address before: 100074 Xinzhuang, Chang Xin store, Fengtai District, Beijing, No. 400

Patentee before: Beijing Gelin Jingfeng Fireproof Glass Co.,Ltd.

CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20121212

Termination date: 20190512

CF01 Termination of patent right due to non-payment of annual fee