CN102558516B - Preparation method of heat insulation material for laminated glass - Google Patents
Preparation method of heat insulation material for laminated glass Download PDFInfo
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- CN102558516B CN102558516B CN 201110441230 CN201110441230A CN102558516B CN 102558516 B CN102558516 B CN 102558516B CN 201110441230 CN201110441230 CN 201110441230 CN 201110441230 A CN201110441230 A CN 201110441230A CN 102558516 B CN102558516 B CN 102558516B
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Abstract
The invention relates to a preparation method of a heat insulation material for laminated glass, and belongs to the technical field of energy conservation and environmental protection. The preparation method of the heat insulation material for the laminated glass comprises the following steps of material feeding, esterification reaction, polycondensation reaction and material discharge. The heat insulation material for the laminated glass, which is prepared by adopting the preparation method provided by the invention, has excellent visible light transmission performance and good heat insulation performance, the whole process can be realized only by using one closed reactor, the production time can be shortened and the production efficiency can be improved; and besides, the process can be realized only by adopting commercial raw materials with low quality control difficulty, so that the cost is low.
Description
Technical field
The present invention relates to a kind of preparation method of heat insulation material for laminated glass, belong to the energy-conserving and environment-protective technical field.
Background technology
Generally, laminated glass is by least one pair of sheet glass, between adopt tackiness agent to make them stacked integrated and form as intermediate coat.Because laminated glass has good safety performance, be widely used in the window glasss such as automobile, aircraft, buildings.But traditional laminated glass can not be heat insulation, this is subject to certain restrictions its application.
As everyone knows, solar ray mainly is comprised of ultraviolet ray, visible ray, infrared rays three parts, its middle-ultraviolet lamp refers to that wavelength is less than the light of 200nm, and visible ray refers to that wavelength is between the light between 200nm to 780nm, and infrared rays refers to and is greater than the light that wavelength is greater than 780nm.In this three parts light, wavelength accounts for the nearly 45% of solar ray total energy between the near infrared energy of 780nm to 2500nm, and this part light is also referred to as invisible heat.Some heat insulation material for laminated glass that can see through visible ray and stop near infrared ray to see through occurred at present, the intermediate coat using this lagging material as laminated glass, just can make laminated glass possess heat insulating function.
Through retrieval, find, the Chinese invention patent that the patent No. is 02814435.X discloses a kind of energy and has seen through visible ray and shield near infrared intermediate film for laminated glasses, its preparation method is: the synthesizing polyethylene butyral, prepare dispersed plasticizer, again with batch mixing with rolling machine by both melting mixings, finally use the pressure forming machine extrusion forming.The Chinese invention patent that the patent No. is 200480038407.8 discloses a kind of energy and has seen through visible ray and shield near infrared intermediate film for laminated glasses, its preparation method is: modulation ITO micro-dispersed liquid, the synthesizing polyethylene butyral, use again mixing roll mixing, finally be shaped with press-forming machine.But, the problem that above-mentioned two preparation methods exist is: synthesis step and mixing step adopt different equipment to complete, and can't be combined, and not only can take too much factory building space, also can cause the production time long because step can't merge, can't enhance productivity.
The Chinese invention patent that the patent No. is 200580017451.5 discloses a kind of energy and has seen through visible ray and shield near infrared laminated film, its preparation method is: choose thermoplastic resin A and thermoplastic resin B, become molten state with forcing machine at high temperature respectively, obtain laminate with the feed die mix flow again, last supplying opening mould, be shaped to sheet.The problem that this preparation method exists is: thermoplastic resin used is commercially available finished product, guarantee to make laminated film and there is the just necessary good commercially available thermoplastic resin of functional quality of performance preferably, and the quality control difficulty of thermoplastic resin is higher, price is also very high certainly for the measured commercially available thermoplastic resin of matter, and this will certainly make the cost of laminated film high.
Summary of the invention
Technical problem to be solved by this invention is: overcome the problem that prior art exists, the preparation method of the heat insulation material for laminated glass that a kind of Preparation equipment is simple, production efficiency is high, with low cost is provided.
The technical scheme that the present invention solves its technical problem is as follows:
The preparation method of heat insulation material for laminated glass, is characterized in that, comprises the following steps:
(1) step that feeds intake: raw materials by weight portion is added in closed reactor, described raw material comprises: phthalic acid 5-20 part, terephthalic acid 5-20 part, hexanodioic acid 10-35 part, ethylene glycol 30-70 part, nano antimony tin oxide or nano-indium stannum oxide slurry 1-25 part; Then, the material stirring in reactor is even;
(2) step of esterification: the heating closed reactor reaches temperature of charge and remains on 120 ℃-180 ℃, carries out esterification, stirs material in reaction process; When the reaction times reached for first scheduled time, obtain the esterification material; Described first scheduled time is more than or equal to 1 hour;
(3) polycondensation steps: reactor is vacuumized, and the heating closed reactor reaches the esterification temperature of charge and remains on 220 ℃-280 ℃, carries out polycondensation, stirs the esterification material in reaction process; When the reaction times reached for second scheduled time, stop heating, obtain the polycondensation material; Described second scheduled time is more than or equal to 3 hours;
(4) discharging step: when the polycondensation temperature of charge is down to 90 ℃-150 ℃, the polycondensation material is discharged to reactor, obtain transparent viscous liquid, i.e. heat insulation material for laminated glass.
The present invention further perfect technical scheme is as follows:
1, in (1) step, the mass fraction of solids of described nano antimony tin oxide or nano-indium stannum oxide slurry is 10-35%, and the mean particle size of nano antimony tin oxide or nano-indium stannum oxide is 10-50nm;
2, in (1) step, also comprise the catalytic antimony trioxide in described raw material, its weight accounts for the 0.1-1 ‰ of raw material gross weight;
3, in (2) step, in esterification forward reaction device, be filled with nitrogen, when the reaction times reached for first scheduled time, stop being filled with nitrogen;
4, when the reaction times of (3) step reach second scheduled time or when (4) step when the polycondensation temperature of charge is down to 90 ℃-150 ℃, reactor unloads vacuum;
5, in (2) step, heat temperature raising speed is 2-5 ℃/minute, and the heat temperature raising time is 30-50 minute; In (3) step, heat temperature raising speed is 3-5 ℃/minute, and the heat temperature raising time is 20-30 minute;
6,, in (2) step, the preferable range of first scheduled time is 1-3 hour; In (3) step, the preferable range of second scheduled time is 3-5 hour;
7,, in (1) step, stir speed (S.S.) is 30-50 rev/min; In (2) step, stir speed (S.S.) is 30-50 rev/min; In (3) step, stir speed (S.S.) is 40-60 rev/min; In (4) step, stir the polycondensation material in temperature-fall period, stir speed (S.S.) is 40-80 rev/min.
The heat insulation material for laminated glass visible light permeability energy that preparation method of the present invention makes is good and have good heat-proof quality, and whole technique only needs a closed reactor just can realize, can shorten the production time, enhances productivity; In addition, the lower marketable material of process using Quality Control difficulty of the present invention can realize, with low cost.
The heat insulation material for laminated glass made by the preparation method of aforementioned heat insulation material for laminated glass.
The heat-insulating laminated glass that the lagging material that the preparation method of aforementioned heat insulation material for laminated glass of take makes is intermediate coat.
Above-mentioned lagging material and heat-insulating laminated glass visible light permeability can be good and be had a good heat-proof quality.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.But the invention is not restricted to given example.The raw materials used commercially available product that is of the present invention.
One, prepare heat insulation material for laminated glass
The preparation method of heat insulation material for laminated glass provided by the invention comprises the following steps:
(1) step that feeds intake: raw materials by weight portion is added in closed reactor, described raw material comprises: phthalic acid 5-20 part, terephthalic acid 5-20 part, hexanodioic acid 10-35 part, ethylene glycol 30-70 part, (screening formulation is: phthalic acid 10-15 part for nano antimony tin oxide or nano-indium stannum oxide slurry 1-25 part, terephthalic acid 10-15 part, hexanodioic acid 20-25 part, ethylene glycol 40-60 part, nano antimony tin oxide or nano-indium stannum oxide slurry 5-15 part); Wherein, addition sequence is for to add successively by above-mentioned formula; The mass fraction of solids of nano antimony tin oxide or nano-indium stannum oxide slurry is 10-35% (preferably 15-30%), and the mean particle size of nano antimony tin oxide or nano-indium stannum oxide is 10-50nm (preferably 20-40nm, more preferably 30nm); Also comprise the catalytic antimony trioxide in described raw material, its weight accounts for the 0.1-1 ‰ (preferably 0.3-0.6 ‰) of raw material gross weight;
Then, by the material stirring in reactor even (the preferred 30-50 rev/min of stir speed (S.S.));
(2) step of esterification: in reactor, be filled with nitrogen, the heating closed reactor reaches temperature of charge and remains on 120 ℃-180 ℃ (preferably 140 ℃-160 ℃), carry out esterification, stir material (stirring for lasting while specifically implementing) in reaction process; Wherein, heat temperature raising speed preferred 2-5 ℃/minute, preferred 30-50 minute of heat temperature raising time, the preferred 30-50 rev/min of stir speed (S.S.);
When the reaction times reached for first scheduled time, stop being filled with nitrogen, obtain the esterification material; Wherein, first scheduled time was more than or equal to 1 hour (preferably 1-3 hour, more preferably 1.5-2 hour); Reacting phenomenon now is: in the receiving bottle of reactor, absence of liquid steams, liquid clarification in reactor.
(3) polycondensation steps: reactor is vacuumized, the heating closed reactor reaches the esterification temperature of charge and remains on 220 ℃-280 ℃ (preferably 240 ℃-260 ℃), carry out polycondensation, stir esterification material (stirring for lasting while specifically implementing) in reaction process; Wherein, heat temperature raising speed preferred 3-5 ℃/minute, preferred 20-30 minute of heat temperature raising time, the preferred 40-60 rev/min of stir speed (S.S.);
When the reaction times reached for second scheduled time, stop heating, obtain the polycondensation material; Wherein, second scheduled time was more than or equal to 3 hours (preferably 3-5 hour);
(4) discharging step: when the polycondensation temperature of charge is down to 90 ℃-150 ℃ (preferably 110 ℃-130 ℃), the polycondensation material is discharged to reactor, obtain transparent viscous liquid, i.e. heat insulation material for laminated glass; Wherein, stir polycondensation material (stirring for lasting while specifically implementing) in temperature-fall period, the preferred 40-80 rev/min of stir speed (S.S.), the heat insulation material for laminated glass obtained is transparent viscous liquid.
Wherein, when the reaction times of (3) step reach second scheduled time or when (4) step when the polycondensation temperature of charge is down to 90 ℃-150 ℃, reactor unloads vacuum.
In the present invention, nano antimony tin oxide (ATO) or nano-indium stannum oxide (ITO) slurry are made by nano antimony tin oxide (ATO) and ethylene glycol or nano-indium stannum oxide (ITO) and ethylene glycol.
The applicant finds after deliberation, adopt the form of nano antimony tin oxide (ATO) or nano-indium stannum oxide (ITO) slurry, can guarantee that nano ATO or nano-ITO have appropriate dispersiveness in the lagging material that makes of application preparation method of the present invention, thereby greatly improve heat preservation and insulation, the mechanical property of the lagging material that application preparation method of the present invention makes.In addition, the mass fraction of solids of slurry is necessary for 10-35%, if too low, nano ATO or the nano-ITO content that can make to apply in the lagging material that preparation method of the present invention makes are too low, and its heat-proof quality can't be met the demands; If too high, the transparency that can make on the one hand to apply the lagging material that preparation method of the present invention makes reduces, affect the visible light permeability energy of laminated glass, dispersiveness in the lagging material that can make on the other hand nano ATO or nano-ITO make in application preparation method of the present invention reduces, and can't give full play to nano ATO or nano-ITO and shield near infrared function.
The invention provides 32 embodiment, the parameter of each embodiment (1) step is listed in table 1, and the parameter of (2) step is listed in table 2, and the parameter of (3) step is listed in table 3, and the parameter of (4) step is listed in table 4.
The lagging material that each embodiment is made is made the film that thickness is 0.5-0.8mm, adopts this area routine techniques to measure its performance perameter, and result is as shown in table 5.Experimental data shows, the visible ray of each film (wavelength 380-720nm) transmitance is 70-85%, and near infrared ray (wavelength 720-2500nm) shielding rate is 60-85%, and visible light permeability can be good and be had a good heat-proof quality.
The parameter of each embodiment (1) step of table 1
The parameter of each embodiment (2) step of table 2
| Table 2 | Temperature of charge (℃) | Temperature rise rate (℃/minute) | Heating-up time (minute) | Stir speed (S.S.) (rev/min) | First scheduled time (hour) |
| Embodiment 1 | 120 | 2 | 50 | 30 | 3 |
| Embodiment 2 | 155 | 4 | 34 | 30 | 1 |
| Embodiment 3 | 125 | 3 | 35 | 30 | 2.5 |
| Embodiment 4 | 150 | 4 | 33 | 30 | 1.5 |
| Embodiment 5 | 165 | 4 | 36 | 30 | 1 |
| Embodiment 6 | 130 | 3 | 37 | 40 | 2 |
| Embodiment 7 | 180 | 5 | 32 | 40 | 2.5 |
| Embodiment 8 | 170 | 4 | 38 | 40 | 1.5 |
| Embodiment 9 | 135 | 3 | 38 | 40 | 3 |
| Embodiment 10 | 175 | 5 | 31 | 40 | 1 |
| Embodiment 11 | 160 | 3 | 47 | 50 | 2 |
| Embodiment 12 | 140 | 4 | 30 | 50 | 1.5 |
| Embodiment 13 | 145 | 4 | 31 | 50 | 3 |
| Embodiment 14 | 180 | 4 | 40 | 50 | 2 |
| Embodiment 15 | 128 | 3 | 36 | 50 | 2.5 |
| Embodiment 16 | 180 | 4 | 40 | 30 | 3 |
| Embodiment 17 | 120 | 2 | 50 | 30 | 2 |
| Embodiment 18 | 134 | 3 | 38 | 30 | 2.5 |
| Embodiment 19 | 125 | 3 | 35 | 30 | 1.5 |
| Embodiment 20 | 142 | 4 | 31 | 30 | 2 |
| Embodiment 21 | 145 | 4 | 31 | 30 | 1.5 |
| Embodiment 22 | 130 | 3 | 37 | 40 | 1 |
| Embodiment 23 | 135 | 3 | 38 | 40 | 2 |
| Embodiment 24 | 160 | 3 | 47 | 40 | 3 |
| Embodiment 25 | 158 | 3 | 46 | 40 | 2.5 |
| Embodiment 26 | 155 | 4 | 34 | 40 | 2 |
| Embodiment 27 | 170 | 3 | 50 | 50 | 2.5 |
| Embodiment 28 | 167 | 4 | 37 | 50 | 3 |
| Embodiment 29 | 165 | 4 | 36 | 50 | 1.5 |
| Embodiment 30 | 140 | 3 | 40 | 50 | 2 |
| Embodiment 31 | 175 | 5 | 31 | 50 | 1 |
| Embodiment 32 | 150 | 3 | 43 | 30 | 1.5 |
The parameter of each embodiment (3) step of table 3
| Table 3 | The esterification temperature of charge (℃) | Temperature rise rate (℃/minute) | Heating-up time (minute) | Stir speed (S.S.) (rev/min) | Second scheduled time (hour) |
| Embodiment 1 | 270 | 5 | 30 | 40 | 3.5 |
| Embodiment 2 | 220 | 3 | 22 | 40 | 3 |
| Embodiment 3 | 225 | 5 | 20 | 40 | 4.5 |
| Embodiment 4 | 240 | 3 | 30 | 40 | 4 |
| Embodiment 5 | 230 | 3 | 22 | 40 | 3 |
| Embodiment 6 | 241 | 5 | 22 | 50 | 5 |
| Embodiment 7 | 235 | 2 | 28 | 50 | 4 |
| Embodiment 8 | 257 | 4 | 22 | 50 | 3.5 |
| Embodiment 9 | 245 | 5 | 22 | 50 | 5 |
| Embodiment 10 | 250 | 3 | 25 | 50 | 4.5 |
| Embodiment 11 | 250 | 4 | 23 | 60 | 3 |
| Embodiment 12 | 260 | 5 | 24 | 60 | 3.5 |
| Embodiment 13 | 255 | 4 | 28 | 60 | 4 |
| Embodiment 14 | 280 | 4 | 25 | 60 | 4.5 |
| Embodiment 15 | 240 | 5 | 22 | 60 | 5 |
| Embodiment 16 | 275 | 4 | 24 | 40 | 3.5 |
| Embodiment 17 | 230 | 4 | 28 | 40 | 3 |
| Embodiment 18 | 269 | 5 | 27 | 40 | 4.5 |
| Embodiment 19 | 220 | 4 | 24 | 40 | 4 |
| Embodiment 20 | 260 | 4 | 30 | 40 | 4.5 |
| Embodiment 21 | 250 | 5 | 21 | 40 | 5 |
| Embodiment 22 | 265 | 5 | 27 | 50 | 3.5 |
| Embodiment 23 | 255 | 4 | 30 | 50 | 3 |
| Embodiment 24 | 235 | 3 | 25 | 50 | 4.5 |
| Embodiment 25 | 220 | 3 | 21 | 50 | 4 |
| Embodiment 26 | 250 | 4 | 24 | 50 | 3.5 |
| Embodiment 27 | 245 | 3 | 25 | 60 | 5 |
| Embodiment 28 | 230 | 3 | 21 | 60 | 4.5 |
| Embodiment 29 | 260 | 4 | 24 | 60 | 3 |
| Embodiment 30 | 260 | 5 | 24 | 60 | 3.5 |
| Embodiment 31 | 225 | 2 | 25 | 60 | 4 |
| Embodiment 32 | 240 | 4 | 23 | 40 | 5 |
The parameter of each embodiment (4) step of table 4
| Table 4 | Be down to temperature (℃) | Stir speed (S.S.) (rev/min) |
| Embodiment 1 | 90 | 40 |
| Embodiment 2 | 135 | 50 |
| Embodiment 3 | 100 | 60 |
| Embodiment 4 | 120 | 70 |
| Embodiment 5 | 125 | 80 |
| Embodiment 6 | 110 | 50 |
| Embodiment 7 | 115 | 60 |
| Embodiment 8 | 120 | 70 |
| Embodiment 9 | 105 | 80 |
| Embodiment 10 | 130 | 60 |
| Embodiment 11 | 110 | 60 |
| Embodiment 12 | 130 | 70 |
| Embodiment 13 | 95 | 80 |
| Embodiment 14 | 140 | 60 |
| Embodiment 15 | 145 | 60 |
| Embodiment 16 | 150 | 40 |
| Embodiment 17 | 135 | 40 |
| Embodiment 18 | 90 | 50 |
| Embodiment 19 | 125 | 60 |
| Embodiment 20 | 100 | 70 |
| Embodiment 21 | 110 | 80 |
| Embodiment 22 | 115 | 50 |
| Embodiment 23 | 120 | 60 |
| Embodiment 24 | 105 | 70 |
| Embodiment 25 | 130 | 80 |
| Embodiment 26 | 120 | 60 |
| Embodiment 27 | 140 | 60 |
| Embodiment 28 | 95 | 70 |
| Embodiment 29 | 130 | 80 |
| Embodiment 30 | 110 | 60 |
| Embodiment 31 | 150 | 60 |
| Embodiment 32 | 120 | 40 |
The performance perameter of each film of table 5
| Table 5 | Thickness (mm) | Visible light transmissivity (%) | Near-infrared shielding rate (%) |
| Embodiment 1 | 0.5 | 85 | 72 |
| Embodiment 2 | 0.7 | 73 | 85 |
| Embodiment 3 | 0.8 | 78 | 80 |
| Embodiment 4 | 0.6 | 79 | 78 |
| Embodiment 5 | 0.6 | 78 | 74 |
| Embodiment 6 | 0.6 | 76 | 85 |
| Embodiment 7 | 0.7 | 80 | 65 |
| Embodiment 8 | 0.5 | 83 | 85 |
| Embodiment 9 | 0.8 | 81 | 78 |
| Embodiment 10 | 0.8 | 70 | 85 |
| Embodiment 11 | 0.5 | 85 | 60 |
| Embodiment 12 | 0.6 | 80 | 70 |
| Embodiment 13 | 0.5 | 85 | 74 |
| Embodiment 14 | 0.7 | 80 | 70 |
| Embodiment 15 | 0.6 | 79 | 72 |
| Embodiment 16 | 0.6 | 80 | 73 |
| Embodiment 17 | 0.7 | 79 | 73 |
| Embodiment 18 | 0.5 | 85 | 81 |
| Embodiment 19 | 0.8 | 72 | 85 |
| Embodiment 20 | 0.8 | 73 | 85 |
| Embodiment 21 | 0.5 | 85 | 85 |
| Embodiment 22 | 0.5 | 85 | 60 |
| Embodiment 23 | 0.7 | 76 | 85 |
| Embodiment 24 | 0.6 | 82 | 72 |
| Embodiment 25 | 0.6 | 82 | 71 |
| Embodiment 26 | 0.5 | 85 | 65 |
| Embodiment 27 | 0.7 | 78 | 80 |
| Embodiment 28 | 0.5 | 85 | 70 |
| Embodiment 29 | 0.6 | 80 | 76 |
| Embodiment 30 | 0.8 | 75 | 85 |
| Embodiment 31 | 0.8 | 80 | 81 |
| Embodiment 32 | 0.8 | 80 | 83 |
Two, prepare heat-insulating laminated glass
The preparation method that the embodiment of first part of take makes the heat-insulating laminated glass that heat insulation material for laminated glass is intermediate coat comprises the following steps: one of (1) aforementioned each embodiment makes heat insulation material for laminated glass;
(2) adopt warming-up device, the sheet glass that is 1-10cm (preferably 3-6cm) by thickness is heated to 70 ℃-90 ℃ (preferably 80 ℃);
(3) on sheet glass heat insulation material for laminated glass uniform spreading to a piece heated, then the sheet glass that another piece was heated is placed on it; Then adopt pressure exerting device that these two sheet glass are compressed; After cooling, obtain heat-insulating laminated glass.
As stated above, take aforementioned 32 heat-insulating laminated glass that embodiment gained lagging material is intermediate coat, its performance perameter is as shown in table 6, and each heat-insulating laminated glass visible light permeability can be good and be had a good heat-proof quality.
The performance perameter of each heat-insulating laminated glass of table 6
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of requirement of the present invention.
Claims (10)
1. the preparation method of heat insulation material for laminated glass, is characterized in that, comprises the following steps:
(1) step that feeds intake: raw materials by weight portion is added in closed reactor, described raw material comprises: phthalic acid 5-20 part, terephthalic acid 5-20 part, hexanodioic acid 10-35 part, ethylene glycol 30-70 part, nano antimony tin oxide or nano-indium stannum oxide slurry 1-25 part; The mass fraction of solids of described nano antimony tin oxide or nano-indium stannum oxide slurry is 10-35%; Then, the material stirring in reactor is even;
(2) step of esterification: the heating closed reactor reaches temperature of charge and remains on 120 ℃-180 ℃, carries out esterification, stirs material in reaction process; When the reaction times reached for first scheduled time, obtain the esterification material; Described first scheduled time is more than or equal to 1 hour;
(3) polycondensation steps: reactor is vacuumized, and the heating closed reactor reaches the esterification temperature of charge and remains on 220 ℃-280 ℃, carries out polycondensation, stirs the esterification material in reaction process; When the reaction times reached for second scheduled time, stop heating, obtain the polycondensation material; Described second scheduled time is more than or equal to 3 hours;
(4) discharging step: when the polycondensation temperature of charge is down to 90 ℃-150 ℃, the polycondensation material is discharged to reactor, obtain transparent viscous liquid, i.e. heat insulation material for laminated glass.
2. the preparation method of heat insulation material for laminated glass according to claim 1, is characterized in that, in (1) step, the mean particle size of nano antimony tin oxide or nano-indium stannum oxide is 10-50nm.
3. the preparation method of heat insulation material for laminated glass according to claim 1, is characterized in that, in (1) step, also comprises the catalytic antimony trioxide in described raw material, and its weight accounts for the 0.1-1 ‰ of raw material gross weight.
4. according to the preparation method of claim 1 or 2 or 3 described heat insulation material for laminated glass, it is characterized in that, in (2) step, in esterification forward reaction device, be filled with nitrogen, when the reaction times reached for first scheduled time, stop being filled with nitrogen.
5. according to the preparation method of claim 1 or 2 or 3 described heat insulation material for laminated glass, it is characterized in that, when the reaction times of (3) step reach second scheduled time or when (4) step when the polycondensation temperature of charge is down to 90 ℃-150 ℃, reactor unloads vacuum.
6. according to the preparation method of claim 1 or 2 or 3 described heat insulation material for laminated glass, it is characterized in that, in (2) step, heat temperature raising speed is 2-5 ℃/minute, and the heat temperature raising time is 30-50 minute; In (3) step, heat temperature raising speed is 3-5 ℃/minute, and the heat temperature raising time is 20-30 minute.
7. according to the preparation method of claim 1 or 2 or 3 described heat insulation material for laminated glass, it is characterized in that, in (2) step, the scope of first scheduled time is 1-3 hour; In (3) step, the scope of second scheduled time is 3-5 hour.
8. according to the preparation method of claim 1 or 2 or 3 described heat insulation material for laminated glass, it is characterized in that, in (1) step, stir speed (S.S.) is 30-50 rev/min; In (2) step, stir speed (S.S.) is 30-50 rev/min; In (3) step, stir speed (S.S.) is 40-60 rev/min; In (4) step, stir the polycondensation material in temperature-fall period, stir speed (S.S.) is 40-80 rev/min.
9. the heat insulation material for laminated glass made by the preparation method of the described heat insulation material for laminated glass of claim 1.
10. the heat-insulating laminated glass that the lagging material that the preparation method of the described heat insulation material for laminated glass of claim 1 of take makes is intermediate coat.
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