CN102746495A - Composite material for preparing infrared barrier polyester film and preparation method thereof - Google Patents

Composite material for preparing infrared barrier polyester film and preparation method thereof Download PDF

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CN102746495A
CN102746495A CN2012102600434A CN201210260043A CN102746495A CN 102746495 A CN102746495 A CN 102746495A CN 2012102600434 A CN2012102600434 A CN 2012102600434A CN 201210260043 A CN201210260043 A CN 201210260043A CN 102746495 A CN102746495 A CN 102746495A
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reaction kettle
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terepthaloyl moietie
composite material
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CN102746495B (en
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陈楚伟
陈晓青
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Central South University
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Abstract

The invention provides a composite material for preparing an infrared barrier polyester film and a preparation method of the composite material. The composite material is prepared from the raw materials: dimethyl terephthalate, nano ceramic powder, a surface treating agent, ground resin, a catalyst and ethylene glycol. The polymer organic-inorganic composite material is prepared by surface treatment, grinding and dispersing, mixing at high speed and high temperature, polymerization and other links. The polyester film prepared from the composite material has the thickness of 23-75mum, has the visible light transmittance about 70%, forms at least 55% infrared barrier effect within the range of infrared spectrum 780-2500nm covered by solar spectrum, and can realize more than 75% infrared barrier effect in the infrared band of 1400-2500nm.

Description

A kind ofly be used to prepare infrared rays and intercept matrix material of polyester film and preparation method thereof
Technical field
The present invention relates to a kind ofly be used to prepare infrared rays and intercept matrix material of polyester film and preparation method thereof.
Background technology
Along with the extensive utilization of nano material in glass art.Automobile and heat-insulating film product continue to bring out.And pet film (being the PET film) is widely used in the thermal insulation film field as the main loading material of thermal insulation film.But consult a large amount of correlation technique data; The method of using realizes through the mode that on transparent polyester film base material, is coated with often, or directly carries out mechanically mixing to the hot-melt object of the dispersion liquid of nano ceramics oxide compound and polyethylene terephthalate.
Though coating process is a kind of comparatively simple technical implementation way.But some is not enough below in use also having highlighted: the first, and weather resistance is difficult to practical requirement; The second, later stage utilization technology is comparatively complicated; The 3rd, be not easy to obtain the planeness high product through the mode that is coated with; The 4th, because the loss that complex process causes has directly improved the cost of product; Directly mix and exist a large amount of non-uniform phenomenons to the nano ceramics dispersion liquid with the hot-melt object of polyester.
Summary of the invention
The object of the invention aims to provide a kind of matrix material; The infrared rays that is made by this material intercepts the scope of polyester film at the infrared spectrum broad of solar spectrum; Can reach good infrared barrier effect, more can realize infrared barrier effect very efficiently at the infrared band of 1400nm to 2500nm.Another object of the present invention aims to provide the preparation method of above-mentioned matrix material.
Matrix material of the present invention comprises that following weight part raw material processes:
Figure BDA00001931450100021
Described surface treatment agent is one or more in 3-methacryloxypropyl trimethoxy silane, sec.-propyl two oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanic acid ester, sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester, tetra isopropyl two (the dioctyl phosphorous acid acyloxy) titanic acid ester;
Described resin is a kind of or its mixture that contains in Hydroxylated acrylic resin, vibrin and the Vinylite;
Described catalyzer is selected from one or more in antimony, tin, sb oxide, the tin-oxide.
Described nano-ceramic powder is a kind of or its mixture in AZO nanometer Al-Doped ZnO powder, ITO nanometer tin-doped indium oxide powder, Nano titanium nitride powder and the nanometer lanthanum hexaborane.
Infrared spectrum 780~2500nm scope that material of the present invention is contained at solar spectrum can reach at least 55% infrared barrier effect, more can realize the infrared barrier effect more than 75% at the infrared band of 1400nm to 2500nm.
The present invention relates to following step:
Step 1: get terepthaloyl moietie and put into reaction kettle 1; Add surface treatment agent, add nano ceramic powder again, be controlled at 80~120 ℃ to the temperature of reaction kettle 1; Stir at high-speed shearing machine; Put into sand mill after disposing, add resin, obtain nano ceramics terepthaloyl moietie dispersion liquid after the grinding and retain subsequent use;
Step 2: get DMT. Dimethyl p-benzenedicarboxylate and put into reaction kettle 2, the nano ceramics terepthaloyl moietie dispersion liquid for preparing in the step 1 is added the reaction kettle 2 with cooling for reflux function, add catalyzer, adding terepthaloyl moietie is some; With reaction kettle 2 sealings, charge into rare gas element nitrogen, be heated to 140 ℃~160 ℃, heated and stirred under non-pressurized situation, is brought up to 160 ℃~220 ℃ with reaction kettle 2 temperature, reacts 3~4 hours; Temperature of reaction kettle is brought up between 260~300 ℃, pressure-controlling is at 100~120 handkerchiefs again, and the reaction times is to stop after 2~4 hours, and draw after postcooling, the granulation finished product.
Stirred 10~30 minutes with 2500-3500 commentaries on classics/min high-speed shearing machine in the said step 1.
Under the speed of 600~1200 commentaries on classics/min, grind 12~24h in the said step 1.
Polyester film of the present invention has following advantage with respect to the traditional optical film: can effectively reduce in the film process and reunite and the fuzzy appearance of sending out situation such as mist, material of the present invention has good infrared barrier effect.1) can simplify the film-forming process of traditional optical thermal insulation film greatly through the application of film of the present invention; 2) film just can be accomplished the repeatedly technology all wave band effect of heat insulation that just can possess of traditional product, greatly reduces the cost of thermal insulation film; 3) through the infrared barrier material is accomplished in the polyester film, improved the comprehensive weather resistance of material greatly; 4) film of preparation has reduced the lines problem in the multi-layer coated mode, the quality of the film of raising.
Description of drawings
Fig. 1 is the pattern that the nano ceramic material after embodiment 1 step 1 is handled observes under Electronic Speculum.
Fig. 2 is the pattern that the nano ceramic material after embodiment 6 step 1 are handled observes under Electronic Speculum.
Fig. 3 be step 1 preparation among the embodiment 1 work in-process and ethylene glycol terephthalate 160 ℃ mix after, the pattern of in vial, observing.
Fig. 4 be step 1 preparation among the embodiment 6 work in-process and ethylene glycol terephthalate 160 ℃ mix after, the pattern of in vial, observing.
Raw material in whole process of production all need reach very high translucent effect just can process the optical thin film that is used on the transparent glass, in case side reaction occurs, it is muddy that the observation with the naked eye of then whole transparent system can become.
Embodiment
Below will further set forth the present invention through a series of embodiment, purpose is better to understand content of the present invention and unrestricted protection scope of the present invention.
Comparative Examples 1
Step 1: get 25 kilograms of terepthaloyl moietie and put into 50 liters reaction kettle 1; The silane coupling agent 3-aminopropyl triethoxysilane that adds 0.02 kilogram; Add 1.5 kilograms of nano-ITOs (nanometer tin-doped indium oxide powder) again; Be controlled at 100 ℃ to the temperature of reaction kettle, stirred 30 minutes, put into sand mill after disposing with the high-shear machine of 3000 commentaries on classics/min; Add 1 kilogram of carboxyl acrylic resin, after grinding 24h under the speed of 600 commentaries on classics/min, obtain nano ceramics terepthaloyl moietie dispersion liquid and retain subsequent use;
Step 2: get 30 kilograms of DMT. Dimethyl p-benzenedicarboxylates and put into 100 liters the reaction kettle with cooling for reflux function 2; The nano ceramics terepthaloyl moietie dispersion liquid for preparing in the step 1 is added reaction kettle 2; Add 0.005 kilogram of tin catalyst, add 20 kilograms of terepthaloyl moietie.With the reaction kettle sealing, charge into rare gas element nitrogen, be heated to 160 ℃, after heated and stirred is mixed about 30 minutes, under non-pressurized situation, temperature of reaction kettle is brought up to 220 ℃ of reactions 3 hours; Temperature of reaction kettle is brought up to 260 ℃, and pressure-controlling is at 110 handkerchiefs, and the reaction times is to stop after 2 hours, and draw after postcooling, the granulation finished product.
Work in-process in the Comparative Examples 1 scheme the first step, it is as shown in Figure 1 through electron microscopy observation.With after rutgers mixes, residual species may observe has obvious particulate material on the vial wall in the time of 160 ℃.This will cause film forming the fuzzy situation (like Fig. 3) of sending out mist to occur.
Embodiment 2
Step 1: get 25 kilograms of terepthaloyl moietie and put into 50 liters reaction kettle 1; Titanate coupling agent sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester that adds 0.1 kilogram; Add 1.5 kilograms of nano silicon nitride ti powder again; Be controlled at 100 ℃ to the temperature of reaction kettle, stirred 30 minutes, put into sand mill after disposing with the high-shear machine of 3000 commentaries on classics/min; Add 1.5 kilograms of hydroxy acryl acid resins, after grinding 24h under the speed of 1000 commentaries on classics/min, obtain nano ceramics terepthaloyl moietie dispersion liquid and retain subsequent use;
Step 2: get 30 kilograms of DMT. Dimethyl p-benzenedicarboxylates and put into 100 liters the reaction kettle with cooling for reflux function 2, the nano ceramics terepthaloyl moietie dispersion liquid for preparing in the step 1 is added reaction kettle 2, add 0.008 kilogram of antimony catalyst, add 20 kilograms of terepthaloyl moietie.With the reaction kettle sealing, charge into rare gas element nitrogen, be heated to 160 ℃, after heated and stirred is mixed about 30 minutes, under non-pressurized situation, temperature of reaction kettle is brought up to 220 ℃ of reactions 3 hours; Temperature of reaction kettle is brought up to 280 ℃, and pressure-controlling is at 100 handkerchiefs, and the reaction times is to stop after 2 hours, and draw after postcooling, the granulation finished product.
Work in-process in the embodiment 2 scheme the first steps, it is similar through its effect of electron microscopy observation and Fig. 2.With after rutgers mixes, observation is Clear & Transparent similar with Fig. 4 in the residue on the vial wall in the time of 160 ℃.The thickness of preparing through embodiment 2 is that the polyester film of 23um records through using Shenzhen woods to attend LS101 and two kinds of detectors of LS160 that Science and Technology Ltd. produces; The transmittance of film can reach 68%; The rejection rate of the infrared rays wave band of 950nm is 50%, and the rejection rate of the infrared rays wave band of 1400nm is 75%.
Comparative Examples 3
Step 1: get 25 kilograms of terepthaloyl moietie and put into 50 liters reaction kettle 1; The silane coupling agent 3-glycidyl ether oxygen propyl trimethoxy silicane that adds 0.05 kilogram; Add 1.5 kilograms of nanometer lanthanum hexaborane powder again; Be controlled at 100 ℃ to the temperature of reaction kettle, stirred 30 minutes, put into sand mill after disposing with the high-shear machine of 3000 commentaries on classics/min; Add 0.5 kilogram and contain the carboxy vinyl resin, after grinding 24h under the speed of 800 commentaries on classics/min, obtain nano ceramics terepthaloyl moietie dispersion liquid and retain subsequent use;
Step 2: get 30 kilograms of DMT. Dimethyl p-benzenedicarboxylates and put into 100 liters the reaction kettle with cooling for reflux function 2; The nano ceramics terepthaloyl moietie dispersion liquid for preparing in the step 1 is added reaction kettle 2; Add 0.01 kilogram of antimony oxide catalyst, add 20 kilograms of terepthaloyl moietie.With the reaction kettle sealing, charge into rare gas element nitrogen, be heated to 160 ℃, after heated and stirred is mixed about 30 minutes, under non-pressurized situation, temperature of reaction kettle is brought up to 220 ℃ of reactions 3 hours; Temperature of reaction kettle is brought up to 280 ℃, and pressure-controlling is at 120 handkerchiefs, and the reaction times is to stop after 3 hours, and draw after postcooling, the granulation finished product.
Work in-process in the Comparative Examples 3 scheme the first steps, it is similar through electron microscopy observation and Fig. 1, and a large amount of reunions are arranged.With after rutgers mixes, residual species may observe has obvious particulate material on the vial wall in the time of 160 ℃.It is similar that this will cause film forming to occur bluring situation and Fig. 3 of sending out mist.
Embodiment 4
Step 1: get 25 kilograms of terepthaloyl moietie and put into 50 liters reaction kettle 1; Titanate coupling agent sec.-propyl two oleic acid acyloxy (the dioctyl phosphoric acid acyloxy) titanic acid ester that adds 0.15 kilogram; Add 1 kilogram of ito powder and 0.5 kilogram of AZO again; Be controlled at 100 ℃ to the temperature of reaction kettle, stirred 30 minutes, put into sand mill after disposing with the high-shear machine of 3000 commentaries on classics/min; Add 2 kilograms and contain carboxyl acrylic resin, after grinding 24h under the speed of 1000 commentaries on classics/mim, obtain nano ceramics terepthaloyl moietie dispersion liquid and retain subsequent use;
Step 2: get 30 kilograms of DMT. Dimethyl p-benzenedicarboxylates and put into 100 liters the reaction kettle with cooling for reflux function 2; The nano ceramics terepthaloyl moietie dispersion liquid for preparing in the step 1 is added reaction kettle 2; Add 0.02 kilogram of tin oxide catalysts, add 20 kilograms of terepthaloyl moietie.With the reaction kettle sealing, charge into rare gas element nitrogen, be heated to 160 ℃, after heated and stirred is mixed about 30 minutes, under non-pressurized situation, temperature of reaction kettle is brought up to 220 ℃ of reactions 3 hours; Temperature of reaction kettle is brought up to 270 ℃, and pressure-controlling is at 120 handkerchiefs, and the reaction times is to stop after 2.5 hours, and draw after postcooling, the granulation finished product.
Work in-process in the embodiment 4 scheme the first steps, it is similar through its effect of electron microscopy observation and Fig. 2.In the time of 160 ℃ with after rutgers mixes, observation Clear & Transparent (like Fig. 4) in the residue on the vial wall.The thickness of preparing through embodiment 4 is that the polyester film of 23um records through using Shenzhen woods to attend LS101 and two kinds of detectors of LS160 that Science and Technology Ltd. produces; The transmittance of film can reach 72%; The rejection rate of the infrared rays wave band of 950nm is 60%, and the rejection rate of the infrared rays wave band of 1400nm is 85%.
Embodiment 5
Step 1: get 25 kilograms of terepthaloyl moietie and put into 50 liters reaction kettle 1; The silane coupling agent 3-methacryloxypropyl trimethoxy silane that adds 0.08 kilogram); Add 1 kilogram of Nano titanium nitride and 0.5 kilogram of nanometer lanthanum hexaborane powdered mixture again; Be controlled at 100 ℃ to the temperature of reaction kettle, stirred 30 minutes, put into sand mill after disposing with the high-shear machine of 3000 commentaries on classics/min; Add 1 kilogram of carboxylic Vinylite, after grinding 24h under the speed of 900 commentaries on classics/min, obtain nano ceramics terepthaloyl moietie dispersion liquid and retain subsequent use;
Step 2: get 30 kilograms of DMT. Dimethyl p-benzenedicarboxylates and put into 100 liters the reaction kettle with cooling for reflux function 2, the nano ceramics terepthaloyl moietie dispersion liquid for preparing in the step 1 is added reaction kettle 2, add 0.005 kilogram of antimony catalyst, add 20 kilograms of terepthaloyl moietie.With the reaction kettle sealing, charge into rare gas element nitrogen, be heated to 160 ℃, after heated and stirred is mixed about 30 minutes, under non-pressurized situation, temperature of reaction kettle is brought up to 220 ℃ of reactions 3 hours; Temperature of reaction kettle is brought up to 260 ℃, and pressure-controlling is at 100 handkerchiefs, and the reaction times is to stop after 3 hours, and draw after postcooling, the granulation finished product.
Execute the work in-process in the routine 5 scheme the first steps, it is similar through its effect of electron microscopy observation and Fig. 2.With after rutgers mixes, observation is Clear & Transparent in the residue on the vial wall, and is similar with Fig. 4 in the time of 160 ℃.The thickness of preparing through embodiment 5 is that the polyester film of 36um records through using Shenzhen woods to attend LS101 and two kinds of detectors of LS160 that Science and Technology Ltd. produces; The transmittance of film can reach 68%; The rejection rate of the infrared rays wave band of 950nm is 75%, and the rejection rate of the infrared rays wave band of 1400nm is 80%.
Embodiment 6
Step 1: get 25 kilograms of terepthaloyl moietie and put into 50 liters reaction kettle 1; Titanate coupling agent tetra isopropyl two (the dioctyl phosphorous acid acyloxy) titanic acid ester that adds 0.05 kilogram); Nano-ITO (nano indium tin oxide) powder that adds 0.5 kilogram of nanometer lanthanum hexaborane and 1 kilogram again; Be controlled at 100 ℃ to the temperature of reaction kettle, stirred 30 minutes, put into sand mill after disposing with the high-shear machine of 3000 commentaries on classics/min; Add 1.5 kilograms of hydroxy acryl acid resins, after grinding 24h under the speed of 1200 commentaries on classics/min, obtain nano ceramics terepthaloyl moietie dispersion liquid and retain subsequent use;
Step 2: get 30 kilograms of DMT. Dimethyl p-benzenedicarboxylates and put into 100 liters the reaction kettle with cooling for reflux function 2; The nano ceramics terepthaloyl moietie dispersion liquid for preparing in the step 1 is added reaction kettle 2; Add 0.015 kilogram of tin oxide catalysts, add 20 kilograms of terepthaloyl moietie.With the reaction kettle sealing, charge into rare gas element nitrogen, be heated to 160 ℃, after heated and stirred is mixed about 30 minutes, under non-pressurized situation, temperature of reaction kettle is brought up to 220 ℃ of reactions 3 hours; Temperature of reaction kettle is brought up to 270 ℃, and pressure-controlling is at 120 handkerchiefs, and the reaction times is to stop after 3 hours, and draw after postcooling, the granulation finished product.
Execute the work in-process in the routine 6 scheme the first steps, it is as shown in Figure 2 through electron microscopy observation.In the time of 160 ℃ with after rutgers mixes, observation Clear & Transparent (like Fig. 4) in the residue on the vial wall.The thickness of preparing through embodiment 6 is that the polyester film of 23um records through using Shenzhen woods to attend LS101 and two kinds of detectors of LS160 that Science and Technology Ltd. produces; The transmittance of film can reach 72%; The rejection rate of the infrared rays wave band of 950nm is 85%, and the rejection rate of the infrared rays wave band of 1400nm is 90%.
Embodiment 7
Step 1: get 25 kilograms of terepthaloyl moietie and put into 50 liters reaction kettle 1; Titanate coupling agent tetra isopropyl two (the dioctyl phosphorous acid acyloxy) titanic acid ester that adds 0.05 kilogram); Add 1.5 kilograms of nano-ITOs (nanometer tin-doped indium oxide powder) again; Be controlled at 100 ℃ to the temperature of reaction kettle, stirred 30 minutes, put into sand mill after disposing with the high-shear machine of 3000 commentaries on classics/min; Add 1.5 kilograms of hydroxy acryl acid resins, after grinding 24h under the speed of 600 commentaries on classics/min, obtain nano ceramics terepthaloyl moietie dispersion liquid and retain subsequent use;
Step 2: get 30 kilograms of DMT. Dimethyl p-benzenedicarboxylates and put into 100 liters the reaction kettle with cooling for reflux function 2; The nano ceramics terepthaloyl moietie dispersion liquid for preparing in the step 1 is added reaction kettle 2; Add 0.005 kilogram of tin catalyst, add 20 kilograms of terepthaloyl moietie.With the reaction kettle sealing, charge into rare gas element nitrogen, be heated to 160 ℃, after heated and stirred is mixed about 30 minutes, under non-pressurized situation, temperature of reaction kettle is brought up to 220 ℃ of reactions 3 hours; Temperature of reaction kettle is brought up to 260 ℃, and pressure-controlling is at 110 handkerchiefs, and the reaction times is to stop after 2 hours, and draw after postcooling, the granulation finished product.
Execute the work in-process in the routine 7 scheme the first steps, it is as shown in Figure 2 through electron microscopy observation.In the time of 160 ℃ with after rutgers mixes, observation Clear & Transparent (like Fig. 4) in the residue on the vial wall.The thickness of preparing through embodiment 7 is that the polyester film of 23um records through using Shenzhen woods to attend LS101 and two kinds of detectors of LS160 that Science and Technology Ltd. produces; The transmittance of film can reach 72%; The rejection rate of the infrared rays wave band of 950nm is 60%, and the rejection rate of the infrared rays wave band of 1400nm is 90%.
Embodiment 8
Step 1: get 25 kilograms of terepthaloyl moietie and put into 50 liters reaction kettle 1; The silane coupling agent 3-methacryloxypropyl trimethoxy silane that adds 0.08 kilogram); The lanthanum hexaborane that adds 1 kilogram of nano silicon nitride ti powder and 0.5 kilogram again; Be controlled at 100 ℃ to the temperature of reaction kettle, stirred 30 minutes, put into sand mill after disposing with the high-shear machine of 3000 commentaries on classics/min; Add 1.5 kilograms of hydroxy acryl acid resins, after grinding 24h under the speed of 1000 commentaries on classics/min, obtain nano ceramics terepthaloyl moietie dispersion liquid and retain subsequent use;
Step 2: get 30 kilograms of DMT. Dimethyl p-benzenedicarboxylates and put into 100 liters the reaction kettle with cooling for reflux function 2, the nano ceramics terepthaloyl moietie dispersion liquid for preparing in the step 1 is added reaction kettle 2, add 0.008 kilogram of antimony catalyst, add 20 kilograms of terepthaloyl moietie.With the reaction kettle sealing, charge into rare gas element nitrogen, be heated to 160 ℃, after heated and stirred is mixed about 30 minutes, under non-pressurized situation, temperature of reaction kettle is brought up to 220 ℃ of reactions 3 hours; Temperature of reaction kettle is brought up to 280 ℃, and pressure-controlling is at 100 handkerchiefs, and the reaction times is to stop after 2 hours, and draw after postcooling, the granulation finished product.
Work in-process in the embodiment 2 scheme the first steps, it is similar through its effect of electron microscopy observation and Fig. 2.With after rutgers mixes, observation is Clear & Transparent similar with Fig. 4 in the residue on the vial wall in the time of 160 ℃.The thickness of preparing through embodiment 2 is that the polyester film of 23um records through using Shenzhen woods to attend LS101 and two kinds of detectors of LS160 that Science and Technology Ltd. produces; The transmittance of film can reach 70%; The rejection rate of the infrared rays wave band of 950nm is 65%, and the rejection rate of the infrared rays wave band of 1400nm is 70%.

Claims (5)

1. one kind is used to prepare the matrix material that infrared rays intercepts polyester film, it is characterized in that, described matrix material comprises that following weight part raw material processes:
Figure FDA00001931450000011
Described surface treatment agent is one or more in 3-methacryloxypropyl trimethoxy silane, sec.-propyl two oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanic acid ester, sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester, tetra isopropyl two (the dioctyl phosphorous acid acyloxy) titanic acid ester;
Described resin is a kind of or its mixture that contains in Hydroxylated acrylic resin, vibrin and the Vinylite;
Described catalyzer is selected from one or more in antimony, tin, sb oxide, the tin-oxide.
2. matrix material according to claim 1 is characterized in that described nano-ceramic powder is a kind of or its mixture in AZO nanometer Al-Doped ZnO powder, ITO nanometer tin-doped indium oxide powder, Nano titanium nitride powder and the nanometer lanthanum hexaborane.
3. the preparation method of claim 1 or 2 described matrix materials is characterized in that, comprises following preparation; Step 1: get part terepthaloyl moietie and put into reaction kettle 1, add surface treatment agent, add nano ceramic powder again; Be controlled at 80~120 ℃ to the temperature of reaction kettle 1, high-speed shearing machine stir, put into sand mill after disposing; Add resin, obtain nano ceramics terepthaloyl moietie dispersion liquid after the grinding and retain subsequent use;
Step 2: get DMT. Dimethyl p-benzenedicarboxylate and put into reaction kettle 2, the nano ceramics terepthaloyl moietie dispersion liquid for preparing in the step 1 is added the reaction kettle 2 with cooling for reflux function, add catalyzer, add remaining terepthaloyl moietie; With reaction kettle 2 sealings, charge into rare gas element nitrogen, be heated to 140 ℃~160 ℃, heated and stirred under non-pressurized situation, is brought up to 160 ℃~220 ℃ with reaction kettle 2 temperature, reacts 3~4 hours; Temperature of reaction kettle is brought up between 260~300 ℃, pressure-controlling is at 100~120 handkerchiefs again, and the reaction times is to stop after 2~4 hours, and draw after postcooling, the granulation finished product.
4. method according to claim 3 is characterized in that, stirs 10~30 minutes with 2500-3500 commentaries on classics/min high-speed shearing machine in the said step 1.
5. method according to claim 3 is characterized in that, under the speed of 600~1200 commentaries on classics/mim, grinds 12~24h in the said step 1.
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CN103113723A (en) * 2013-02-25 2013-05-22 杭州天地数码科技有限公司 Method for finely producing energy-saving transparent film with high infrared thermal insulation rate
CN105001437A (en) * 2015-07-20 2015-10-28 安徽工程大学 Ultraviolet shielding type translucent thermal-insulation film preparation method
CN105001602A (en) * 2015-07-20 2015-10-28 安徽工程大学 PET/LaB6 organic phase nanometer composite film and preparation method thereof
CN105418934A (en) * 2015-12-31 2016-03-23 湖北大学 High-transparency thermal insulation type thermoplasticity poly(ether ester) and preparation method and application thereof
CN106700443A (en) * 2016-12-21 2017-05-24 浙江恒逸高新材料有限公司 Preparation method of high-transparency and anti-ultraviolet polyester
CN112280020A (en) * 2020-10-26 2021-01-29 天津华新盈聚酯材料科技有限公司 Polyester chip for producing ultraviolet-infrared light absorption film and preparation method thereof
CN113736230A (en) * 2021-09-08 2021-12-03 金平实 Degradable functional mulching film and preparation method thereof

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CN102516509A (en) * 2011-11-16 2012-06-27 南京兰埔成实业有限公司 Method for preparing polyester slices for optical film and optical film

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CN101580631A (en) * 2008-09-01 2009-11-18 广东炜林纳功能材料有限公司 Toughened and modified polyethylene terephthalate composite material and preparation method thereof
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CN103113723A (en) * 2013-02-25 2013-05-22 杭州天地数码科技有限公司 Method for finely producing energy-saving transparent film with high infrared thermal insulation rate
CN105001437A (en) * 2015-07-20 2015-10-28 安徽工程大学 Ultraviolet shielding type translucent thermal-insulation film preparation method
CN105001602A (en) * 2015-07-20 2015-10-28 安徽工程大学 PET/LaB6 organic phase nanometer composite film and preparation method thereof
CN105001437B (en) * 2015-07-20 2017-10-03 安徽工程大学 A kind of preparation method of ultraviolet shielded type printing opacity thermal insulation film
CN105418934A (en) * 2015-12-31 2016-03-23 湖北大学 High-transparency thermal insulation type thermoplasticity poly(ether ester) and preparation method and application thereof
CN105418934B (en) * 2015-12-31 2018-05-25 湖北大学 A kind of high transparency heat insulation type thermoplastic polyether ester and its preparation method and application
CN106700443A (en) * 2016-12-21 2017-05-24 浙江恒逸高新材料有限公司 Preparation method of high-transparency and anti-ultraviolet polyester
CN112280020A (en) * 2020-10-26 2021-01-29 天津华新盈聚酯材料科技有限公司 Polyester chip for producing ultraviolet-infrared light absorption film and preparation method thereof
CN112280020B (en) * 2020-10-26 2022-07-22 天津华新盈聚酯材料科技有限公司 Polyester chip for producing ultraviolet-infrared light absorption film and preparation method thereof
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