CN105778067A - Internal addition synthetic composite material of infrared barrier polyester chip and preparation method thereof - Google Patents
Internal addition synthetic composite material of infrared barrier polyester chip and preparation method thereof Download PDFInfo
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- CN105778067A CN105778067A CN201610184795.5A CN201610184795A CN105778067A CN 105778067 A CN105778067 A CN 105778067A CN 201610184795 A CN201610184795 A CN 201610184795A CN 105778067 A CN105778067 A CN 105778067A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/85—Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
- C08G63/86—Germanium, antimony, or compounds thereof
- C08G63/866—Antimony or compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2258—Oxides; Hydroxides of metals of tungsten
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The invention discloses an internal addition synthetic composite material of an infrared barrier polyester chip and a preparation method thereof. The method comprises the following steps of: 1) feeding glycol and terephthalic acid into a pulping kettle so as to prepare a slurry; 2) feeding glycol and antimonous oxide into a catalyst preparation kettle so as to prepare a catalyst solution; 3) mixing an additive with the glycol so as to prepare an additive solution; 4) feeding the slurry and the catalyst solution into an esterification kettle and performing esterification reaction; 5) compressing a compound ester into a pre-condensation kettle, adding the additive solution, vacuumizing during a reaction process and discharging excessive glycol; 6) performing condensation polymerization on pre-condensation products, so as to obtain a melt; 7) and cooling and granulating the melt; and 8) drying and packaging. The infrared barrier polyester chip can be used for directly producing an infrared barrier two-way stretching polyester film, and has a full-waveband infrared barrier ratio not less than 90 percent and visible light transmittance not less than 70 percent.
Description
Technical field
The present invention relates to the interior interpolation synthetic composite material of a kind of infrared barrier polyester slice and preparation method.
Background technology
Infrared barrier polyester slice is the polyester synthesis technology by interior interpolation, a kind of section produced, for being directly produced biaxial tension infrared barrier mylar, and the method being substituted on mylar coating, simplify production technology, reduce production cost, the effect enhanced one's market competitiveness, therefore, wide market.
Summary of the invention
It is an object of the invention to provide the interior interpolation synthetic composite material of a kind of infrared barrier polyester slice and preparation method.
The technical solution used in the present invention is:
A kind of interior interpolation synthetic composite material of infrared barrier polyester slice, it is made up of each raw material of following weight percentage ratio:
Ethylene glycol: 30-40%
P-phthalic acid: 60-70%
Modified Nano tungsten oxide: 0.2-5%
Catalyst: 0.02-0.05%
Remaining for dispersant；
Wherein, described catalyst is any in antimony oxide, organic tin or titanium catalyst, it is preferable that antimony oxide；Described dispersant is any or multiple in stearic acid, methacrylic acid, methyl methacrylate, 2-(Acryloyloxy)ethanol, butyl acrylate；
The preparation method of described modified Nano tungsten oxide comprises the following steps:
1. at 25-35 DEG C, nanometer tungsten oxide, ethanol, stearic acid, surfactant are sufficiently mixed, then dry, grind, obtain powder body；
2. at 25-35 DEG C, upper step gained powder body is joined in ethanol, then in ethanol, adds methacrylic acid, methyl methacrylate, 2-(Acryloyloxy)ethanol, butyl acrylate, initiator, be sufficiently mixed, it is warming up to 68-72 DEG C, insulation 4.5-5.5h, then it is warming up to 75-78 DEG C, it is incubated 1-2h, product is taken out after terminating by reaction, filter after centrifugal, then with ethanol, product is washed, then product is dried；
Step 1. in, the quality of described nanometer tungsten oxide is the 30-40% of ethanol quality；Stearic quality is the 1-2% of nanometer tungsten oxide；The quality of surfactant is the 1-2% of nanometer tungsten oxide；
Step 2. in, described methacrylic acid, methyl methacrylate, 2-(Acryloyloxy)ethanol, butyl acrylate mass ratio be 1:(0.8-1.2): (0.8-1.2): (0.8-1.2)；The quality of described powder body is the 4-5% of ethanol quality, methacrylic acid, methyl methacrylate, 2-(Acryloyloxy)ethanol, 3-4 times that gross mass is powder quality of butyl acrylate, the quality of described initiator is the 0.1-0.5% of the gross mass of methacrylic acid, methyl methacrylate, 2-(Acryloyloxy)ethanol, butyl acrylate, and described initiator is any in azodiisobutyronitrile, dibenzoyl peroxide.
The preparation method of the interior composite adding synthesis of a kind of infrared barrier polyester slice, comprises the following steps:
1) ethylene glycol is put in making beating still, be subsequently adding p-phthalic acid, make serosity；
2) ethylene glycol is put into catalyst preparation still, be subsequently adding catalyst, stir and make catalyst liquid；
3) modified Nano tungsten oxide is mixed with ethylene glycol, make additive liquid；
4) putting in esterifying kettle by serosity, catalyst liquid, heating carries out esterification, obtains carboxylate；
5) carboxylate is pressed in precondensation still after esterification and carries out precondensation, add above-mentioned additive liquid, evacuation in course of reaction, excessive ethylene glycol is discharged；
6) product of precondensation is pressed into whole polycondensation vessel, carries out polycondensation reaction further, obtain melt；
7) by melt cooling, pelletizing；
8) dry, packaging；
The interior interpolation synthetic composite material of a kind of infrared barrier polyester slice and preparation method, described step 1), step 2), step 3) in the amount ratio of ethylene glycol be 15.4-17:1:1.
The interior interpolation synthetic composite material of a kind of infrared barrier polyester slice and preparation method, esterification temperature is 250～255 DEG C, and the response time is 3.5～4.5h.
The interior interpolation synthetic composite material of a kind of infrared barrier polyester slice and preparation method: precondensation temperature is 255～260 DEG C, the response time is 0.8～1.2h.
The interior interpolation synthetic composite material of a kind of infrared barrier polyester slice and preparation method, whole condensation temperature is 280～285 DEG C, and the response time is 4.5-5.0h.
The invention has the beneficial effects as follows:
The infrared barrier polyester slice produced by the present invention can be directly used for manufacturing infrared barrier biaxially oriented polyester film, may replace traditional coating process, simplify production technology, reduce cost, all-waveband infrared rejection rate >=90% of thin film, it is seen that light transmission rate >=70%.
Detailed description of the invention
Embodiment 1:
The interior composite adding synthesis of a kind of infrared barrier polyester slice and preparation method, comprise the following steps:
1) 1540～1700 liters of ethylene glycol are put into making beating still, be subsequently adding 4400kg p-phthalic acid, make serosity；
2) 100 liters of ethylene glycol are put into catalyst preparation still, it is subsequently adding the gross mass accounting for p-phthalic acid and ethylene glycol (namely in whole technique, the gross mass of p-phthalic acid and ethylene glycol) 0.03% antimony oxide, stir and make catalyst liquid；
3) by accounting for the modified Nano tungsten oxide of the p-phthalic acid gross mass (namely in whole technique, the gross mass of p-phthalic acid and ethylene glycol) 0.2% with ethylene glycol, mix with 100 liters of ethylene glycol, make additive liquid；
4) serosity and catalyst liquid being put into esterifying kettle, heating carries out esterification to 250～255 DEG C, is stirred, reacts 3.5～4.5h, obtain carboxylate in the process of reaction；
5) after esterification, carboxylate is pressed into preshrunk still, adds additive liquid, heat to 255～260 DEG C of reaction 0.8～1.2h, evacuation in course of reaction, excessive ethylene glycol is discharged；
6) product of precondensation being pressed into whole polycondensation vessel, heating, to 280～285 DEG C, is reacted 4.5～5.0 hours, is obtained infrared barrier polyester fondant；
7) by melt cooling, pelletizing；
8) dry, packaging.
Wherein, additive agent modified nanometer tungsten oxide is prepared: 1. at 35 DEG C, nanometer tungsten oxide, ethanol, stearic acid, surfactant sodium dodecyl base benzene sulfonic acid sodium salt is sufficiently mixed, dry at 120 DEG C, grinds, obtains powder body；2. at 25 DEG C, upper step gained powder body is added in ethanol, then in ethanol, adds methacrylic acid, methyl methacrylate, 2-(Acryloyloxy)ethanol, butyl acrylate, initiator A IBN, be sufficiently mixed, it is warming up to 72 DEG C, insulation 4.5h, then it is warming up to 78 DEG C, it is incubated 1h, product is taken out after terminating by reaction, filter after centrifugal, then with ethanol, product is washed, then product is dried；Step 1. in, the quality of described nanometer tungsten oxide is the 30% of ethanol quality；Stearic quality is the 1% of nanometer tungsten oxide；Quality is nanometer tungsten oxide the 1% of surfactant sodium dodecyl base benzene sulfonic acid sodium salt；Step 2. in, described methacrylic acid, methyl methacrylate, 2-(Acryloyloxy)ethanol, butyl acrylate mass ratio be 1:0.8:0.8:0.8；The quality of described powder body is the 4% of ethanol quality, methacrylic acid, methyl methacrylate, 2-(Acryloyloxy)ethanol, gross mass is powder quality 3 times of butyl acrylate, the quality of described initiator is the 0.1% of the gross mass of methacrylic acid, methyl methacrylate, 2-(Acryloyloxy)ethanol, butyl acrylate.
Embodiment 2:
The interior interpolation synthetic composite material of a kind of infrared barrier polyester slice and preparation method, comprise the following steps:
1) 1540～1700 liters of ethylene glycol are put into making beating still, be subsequently adding 4400kg p-phthalic acid, make serosity；
2) 100 liters of ethylene glycol are put into catalyst preparation still, it is subsequently adding the gross mass accounting for p-phthalic acid and ethylene glycol (namely in whole technique, the gross mass of p-phthalic acid and ethylene glycol) 0.04% antimony oxide, stir and make catalyst liquid；
3) by accounting for the modified Nano tungsten oxide of the p-phthalic acid gross mass (namely in whole technique, the gross mass of p-phthalic acid and ethylene glycol) 2% with ethylene glycol, mix with 100 liters of ethylene glycol, make additive liquid；
4) serosity and catalyst liquid being put into esterifying kettle, heating carries out esterification to 250～255 DEG C, is stirred, reacts 3.5～4.5h, obtain carboxylate in the process of reaction；
5) after esterification, carboxylate is pressed into preshrunk still, adds additive liquid, heat to 255～260 DEG C of reaction 0.8～1.2h, evacuation in course of reaction, excessive ethylene glycol is discharged；
6) product of precondensation being pressed into whole polycondensation vessel, heating, to 280～285 DEG C, is reacted 4.5～5.0 hours, is obtained infrared barrier polyester fondant；
7) by melt cooling, pelletizing；
8) dry, packaging.
Wherein, additive agent modified nanometer tungsten oxide is prepared: 1. at 25 DEG C, nanometer tungsten oxide, ethanol, stearic acid, surfactant sodium dodecyl base benzene sulfonic acid sodium salt is sufficiently mixed, dry at 100 DEG C, grinds, obtains powder body；2. at 25 DEG C, upper step gained powder body is added in ethanol, then in ethanol, adds methacrylic acid, methyl methacrylate, 2-(Acryloyloxy)ethanol, butyl acrylate, initiator A IBN, be sufficiently mixed, it is warming up to 72 DEG C, insulation 5h, then it is warming up to 78 DEG C, it is incubated 1.5h, product is taken out after terminating by reaction, filter after centrifugal, then with ethanol, product is washed, then product is dried；Step 1. in, the quality of described nanometer tungsten oxide is the 35% of ethanol quality；Stearic quality is the 1.5% of nanometer tungsten oxide；Quality is nanometer tungsten oxide the 1.5% of surfactant sodium dodecyl base benzene sulfonic acid sodium salt；Step 2. in, described methacrylic acid, methyl methacrylate, 2-(Acryloyloxy)ethanol, butyl acrylate mass ratio be 1:1:1:1；The quality of described powder body is the 4.5% of ethanol quality, methacrylic acid, methyl methacrylate, 2-(Acryloyloxy)ethanol, gross mass is powder quality 3.5 times of butyl acrylate, the quality of described initiator is the 0.3% of the gross mass of methacrylic acid, methyl methacrylate, 2-(Acryloyloxy)ethanol, butyl acrylate.
Embodiment 3:
The interior composite adding synthesis of a kind of infrared barrier polyester slice and preparation method, comprise the following steps:
1) 1540～1700 liters of ethylene glycol are put into making beating still, be subsequently adding 4400kg p-phthalic acid, make serosity；
2) 100 liters of ethylene glycol are put into catalyst preparation still, it is subsequently adding the gross mass accounting for p-phthalic acid and ethylene glycol (namely in whole technique, the gross mass of p-phthalic acid and ethylene glycol) 0.035% antimony oxide, stir and make catalyst liquid；
3) by accounting for the modified Nano tungsten oxide of the p-phthalic acid gross mass (namely in whole technique, the gross mass of p-phthalic acid and ethylene glycol) 5% with ethylene glycol, mix with 100 liters of ethylene glycol, make additive liquid；
4) serosity and catalyst liquid being put into esterifying kettle, heating carries out esterification to 250～255 DEG C, is stirred, reacts 3.5～4.5h, obtain carboxylate in the process of reaction；
5) after esterification, carboxylate is pressed into preshrunk still, adds additive liquid, heat to 255～260 DEG C of reaction 0.8～1.2h, evacuation in course of reaction, excessive ethylene glycol is discharged；
6) product of precondensation being pressed into whole polycondensation vessel, heating, to 280～285 DEG C, is reacted 4.5～5.0 hours, is obtained amorphous polyester chip；
7) by melt cooling, pelletizing；
8) dry, packaging.
Wherein, additive agent modified nanometer tungsten oxide is prepared: 1. at 35 DEG C, nanometer tungsten oxide, ethanol, stearic acid, surfactant sodium dodecyl base benzene sulfonic acid sodium salt is sufficiently mixed, dry at 120 DEG C, grinds, obtains powder body；2. at 25-35 DEG C, upper step gained powder body is added in ethanol, then in ethanol, adds methacrylic acid, methyl methacrylate, 2-(Acryloyloxy)ethanol, butyl acrylate, initiator B PO, be sufficiently mixed, it is warming up to 72 DEG C, insulation 5.5h, then it is warming up to 78 DEG C, it is incubated 2h, product is taken out after terminating by reaction, filter after centrifugal, then with ethanol, product is washed, then product is dried；Step 1. in, the quality of described nanometer tungsten oxide is the 40% of ethanol quality；Stearic quality is the 2% of nanometer tungsten oxide；Quality is nanometer tungsten oxide the 2% of surfactant sodium dodecyl base benzene sulfonic acid sodium salt；Step 2. in, described methacrylic acid, methyl methacrylate, 2-(Acryloyloxy)ethanol, butyl acrylate mass ratio be 1:1.2:1.2:1.2；The quality of described powder body is the 5% of ethanol quality, methacrylic acid, methyl methacrylate, 2-(Acryloyloxy)ethanol, gross mass is powder quality 4 times of butyl acrylate, the quality of described initiator is the 0.5% of the gross mass of methacrylic acid, methyl methacrylate, 2-(Acryloyloxy)ethanol, butyl acrylate.
Adopt the biaxially oriented polyester film that the embodiment of the present invention 1-3 section prepared is prepared from, all-waveband infrared rejection rate >=90%, it is seen that light transmission rate >=70%.
Claims (6)
1. the interior interpolation synthetic composite material of an infrared barrier polyester slice, it is characterised in that it is made up of each raw material of following weight percentage ratio:
Ethylene glycol: 30-40%
P-phthalic acid: 60-70%
Modified Nano tungsten oxide: 0.2-5%
Catalyst: 0.02-0.05%
Remaining for dispersant；
Wherein, described catalyst is any in antimony oxide, organic tin or titanium catalyst, it is preferable that antimony oxide；Described dispersant is any or multiple in stearic acid, methacrylic acid, methyl methacrylate, 2-(Acryloyloxy)ethanol, butyl acrylate；
The preparation method of described modified Nano tungsten oxide comprises the following steps:
1. at 25-35 DEG C, nanometer tungsten oxide, ethanol, stearic acid, surfactant are sufficiently mixed, then dry, grind, obtain powder body；
2. at 25-35 DEG C, upper step gained powder body is joined in ethanol, then in ethanol, adds methacrylic acid, methyl methacrylate, 2-(Acryloyloxy)ethanol, butyl acrylate, initiator, be sufficiently mixed, it is warming up to 68-72 DEG C, insulation 4.5-5.5h, then it is warming up to 75-78 DEG C, it is incubated 1-2h, product is taken out after terminating by reaction, filter after centrifugal, then with ethanol, product is washed, then product is dried；
Step 1. in, the quality of described nanometer tungsten oxide is the 30-40% of ethanol quality；Stearic quality is the 1-2% of nanometer tungsten oxide；The quality of surfactant is the 1-2% of nanometer tungsten oxide；
Step 2. in, described methacrylic acid, methyl methacrylate, 2-(Acryloyloxy)ethanol, butyl acrylate mass ratio be 1:(0.8-1.2): (0.8-1.2): (0.8-1.2)；The quality of described powder body is the 4-5% of ethanol quality, methacrylic acid, methyl methacrylate, 2-(Acryloyloxy)ethanol, 3-4 times that gross mass is powder quality of butyl acrylate, the quality of described initiator is the 0.1-0.5% of the gross mass of methacrylic acid, methyl methacrylate, 2-(Acryloyloxy)ethanol, butyl acrylate, and described initiator is any in azodiisobutyronitrile, dibenzoyl peroxide.
2. the preparation method of the interior interpolation synthetic composite material of an infrared barrier polyester slice as claimed in claim 1, it is characterised in that comprise the following steps:
1) ethylene glycol is put in making beating still, be subsequently adding p-phthalic acid, make serosity；
2) ethylene glycol is put into catalyst preparation still, be subsequently adding catalyst, stir and make catalyst liquid；
3) modified Nano tungsten oxide is mixed with ethylene glycol, make additive liquid；
4) putting in esterifying kettle by serosity, catalyst liquid, heating carries out esterification, obtains carboxylate；
5) carboxylate is pressed in precondensation still after esterification and carries out precondensation, add above-mentioned additive liquid, evacuation in course of reaction, excessive ethylene glycol is discharged；
6) product of precondensation is pressed into whole polycondensation vessel, carries out polycondensation reaction further, obtain melt；
7) by melt cooling, pelletizing；
8) dry, packaging.
3. the interior interpolation synthetic composite material of a kind of infrared barrier polyester slice according to claim 1,2 and preparation method, it is characterised in that: described step 1), step 2), step 3) in the amount ratio of ethylene glycol be 15.4-17:1:1.
4. the interior interpolation synthetic composite material of a kind of infrared barrier polyester slice according to claim 1,2 and preparation method, it is characterised in that: esterification temperature is 250～255 DEG C, and the response time is 3.5～4.5h.
5. the interior interpolation synthetic composite material of a kind of infrared barrier polyester slice according to claim 1,2 and preparation method, it is characterised in that: precondensation temperature is 255～260 DEG C, and the response time is 0.8～1.2h.
6. the interior interpolation synthetic composite material of a kind of infrared barrier polyester slice according to claim 1,2 and preparation method, it is characterised in that: whole condensation temperature is 280～285 DEG C, and the response time is 4.5-5.0h.
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| CN201610184795.5A CN105778067A (en) | 2016-03-26 | 2016-03-26 | Internal addition synthetic composite material of infrared barrier polyester chip and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108501489A (en) * | 2018-02-02 | 2018-09-07 | 张家港康得新光电材料有限公司 | A kind of primary colors film |
| CN109295532A (en) * | 2018-09-29 | 2019-02-01 | 浙江和也健康科技有限公司 | A kind of antibacterial composite functional fibre and preparation method thereof |
| CN112010771A (en) * | 2020-09-08 | 2020-12-01 | 河北建新化工股份有限公司 | Preparation method of n-hexyl 2- (4-diethylamino-2-hydroxybenzoyl) benzoate |
| CN114479372A (en) * | 2021-12-24 | 2022-05-13 | 江苏双星彩塑新材料股份有限公司 | Polyester film for optical composite film and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108501489A (en) * | 2018-02-02 | 2018-09-07 | 张家港康得新光电材料有限公司 | A kind of primary colors film |
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| CN114479372A (en) * | 2021-12-24 | 2022-05-13 | 江苏双星彩塑新材料股份有限公司 | Polyester film for optical composite film and preparation method thereof |
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Application publication date: 20160720 |