CN112210102A - High-barrier PETG (polyethylene terephthalate glycol) aluminized composite film and preparation method thereof - Google Patents
High-barrier PETG (polyethylene terephthalate glycol) aluminized composite film and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2429/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2429/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2469/00—Characterised by the use of polycarbonates; Derivatives of polycarbonates
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- 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
- C08K3/16—Halogen-containing compounds
- C08K2003/164—Aluminum halide, e.g. aluminium chloride
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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
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- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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Abstract
The invention discloses a high-barrier PETG aluminized composite film and a preparation method thereof, belonging to the technical field of polymer material preparation, wherein the preparation method comprises the steps of putting raw materials for preparing PETG particles into an extruder, and carrying out melt blending granulation to obtain PETG particles; dissolving aluminum chloride in deionized water, performing ultrasonic dispersion, adding a silane coupling agent under the stirring condition, and adjusting the pH of the solution to be acidic to obtain a modified aluminum chloride solution; adding the PETG particles prepared in the step (1) into a mixed solvent of 1,1,2, 2-tetrachloroethane and xylene, mixing, adding an isocyanate type curing agent, heating to completely dissolve the isocyanate type curing agent, and then adding the isocyanate type curing agent into the modified aluminum chloride solution prepared in the step (2) to obtain a casting solution; and dripping the casting film on a glass slide, and placing the glass slide in a vacuum oven until the solvent is completely volatilized to obtain the PETG aluminized composite film.
Description
Technical Field
The invention belongs to the technical field of high polymer material preparation, and particularly relates to a high-barrier PETG (polyethylene terephthalate glycol) aluminized composite film and a preparation method thereof.
Background
PETG is a ternary copolyester, is fully called polyethylene glycol terephthalate-1, 4-cyclohexane dimethanol ester, and is an excellent heat shrinkable film material; wherein the dihydric alcohol monomer is Ethylene Glycol (EG) and 1, 4-Cyclohexanedimethanol (CHDM), the dibasic acid monomer is terephthalic acid (PTA), and when the CHDM content is lower than that of the Ethylene Glycol (EG), namely the mole number of the CHDM in the two dihydric alcohols is less than 50%, the copolyester is PETG, otherwise, the copolyester is PCTG.
PETG is an amorphous copolyester material, and has good transparency, excellent chemical resistance, processability and environmental protection property; with the increasing requirements of people on PETG materials, composite films are continuously developed, and composite nano particles or composite metal ions are developed to a certain degree, but the problems of more complicated preparation steps and unsatisfactory product performance exist.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a high-barrier PETG aluminized composite film which has good mechanical property and barrier property and good application prospect. The invention aims to solve another technical problem of providing a preparation method of the high-barrier PETG aluminized composite film, which has the advantages of simple steps, mild conditions and capability of greatly saving the production efficiency.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a preparation method of a high-barrier PETG aluminized composite film comprises the following steps:
(1) putting the raw materials for preparing the PETG granules into an extruder, and carrying out melt blending granulation to obtain the PETG granules;
(2) dissolving aluminum chloride in deionized water, performing ultrasonic dispersion, adding a silane coupling agent under the stirring condition, and adjusting the pH of the solution to be acidic to obtain a modified aluminum chloride solution;
(3) adding the PETG particles prepared in the step (1) into a mixed solvent of 1,1,2, 2-tetrachloroethane and xylene, mixing, adding an isocyanate type curing agent, heating to completely dissolve the isocyanate type curing agent, and then adding the isocyanate type curing agent into the modified aluminum chloride solution prepared in the step (2) to obtain a casting solution; and dripping the casting film on a glass slide, and putting the glass slide in a vacuum oven until the solvent is completely volatilized to obtain the PETG aluminized composite film.
The preparation method of the high-barrier PETG aluminized composite film comprises the following components in parts by weight: 30-50 parts of PETG resin, 20-30 parts of polyvinyl alcohol, 10-20 parts of polycarbonate and 10-20 parts of styrene.
The preparation method of the high-barrier PETG aluminized composite film comprises the following components in parts by weight: 40-50 parts of PETG resin, 20-25 parts of polyvinyl alcohol, 15-20 parts of polycarbonate and 13-18 parts of styrene.
The preparation method of the high-barrier PETG aluminized composite film comprises the step (1), wherein the extrusion capacity of an extruder is set to be 1300kg/h, the extrusion temperature is 200-300 ℃, the temperature of a machine head is 250 ℃, and the obtained granules are dried until the moisture content is less than 1.5 per mill.
According to the preparation method of the high-barrier PETG aluminized composite film, the temperature of a vacuum oven is 120-150 ℃.
According to the preparation method of the high-barrier PETG aluminized composite film, the silane coupling agent is 3-aminopropyltrimethoxysilane or N, N-bis- (beta-hydroxyethyl) -gamma-aminopropyltriethoxysilane.
According to the preparation method of the high-barrier PETG aluminized composite film, the mass concentration of aluminum ions in the modified aluminum chloride solution is 0.1-1.0%.
The preparation method of the high-barrier PETG aluminized composite film comprises the step (2) that the mass ratio of aluminum chloride to silane coupling agent is 1: 2-1: 4; and adjusting the pH value of the solution to 2-4 by using hydrochloric acid.
According to the preparation method of the high-barrier PETG aluminized composite film, the volume ratio of the 1,1,2, 2-tetrachloroethane to the dimethylbenzene is 1: 1.
The high-barrier PETG aluminized composite film prepared by the preparation method.
Has the advantages that: compared with the prior art, the invention has the advantages that:
(1) the high-barrier PETG aluminized composite film has good mechanical property and barrier property and good application prospect.
(2) The preparation method of the high-barrier PETG aluminized composite film has the advantages of simple steps, mild conditions and capability of greatly saving production efficiency.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
Example 1
A preparation method of a high-barrier PETG aluminized composite film comprises the following steps:
(1) putting 40 parts of PETG resin, 30 parts of polyvinyl alcohol, 10 parts of polycarbonate and 13 parts of styrene into an extruder, melting, blending and granulating to obtain PETG granules, and drying until the moisture content is less than 1.5 per mill for later use; the extrusion capacity of the extruder is set to 1300kg/h, the extrusion temperature is 200 ℃, and the head temperature is 250 ℃;
(2) dissolving aluminum chloride in deionized water, performing ultrasonic dispersion, adding 3-aminopropyltrimethoxysilane under the stirring condition, and adjusting the pH value of the solution to be 2 by using hydrochloric acid to obtain a modified aluminum chloride solution; the mass concentration of aluminum ions in the modified aluminum chloride solution is 0.1 percent; the mass ratio of the aluminum chloride solid to the 3-aminopropyl trimethoxy silane is 1: 2;
(3) adding the PETG particles prepared in the step (1) into a mixed solvent of 1,1,2, 2-tetrachloroethane and xylene (volume ratio is 1: 1), mixing, adding an isocyanate type curing agent, heating to completely dissolve the isocyanate type curing agent, and then adding the isocyanate type curing agent into the modified aluminum chloride solution prepared in the step (2) to obtain a casting solution; and (3) dripping the casting film on the glass slide, placing the glass slide in a vacuum oven, setting the temperature of the vacuum oven at 120 ℃, and drying until the solvent is completely volatilized to obtain the PETG aluminized composite film.
Example 2
A preparation method of a high-barrier PETG aluminized composite film comprises the following steps:
(1) 50 parts of PETG resin, 25 parts of polyvinyl alcohol, 15 parts of polycarbonate and 13 parts of styrene are put into an extruder, melted, blended and granulated to obtain PETG granules, and the PETG granules are dried until the moisture content is less than 1.5 per mill for later use; the extrusion capacity of the extruder is set to 1300kg/h, the extrusion temperature is 300 ℃, and the head temperature is 250 ℃;
(2) dissolving aluminum chloride in deionized water, performing ultrasonic dispersion, adding 3-aminopropyltrimethoxysilane under the stirring condition, and adjusting the pH value of the solution to 4 by using hydrochloric acid to obtain a modified aluminum chloride solution; the mass concentration of aluminum ions in the modified aluminum chloride solution is 0.5 percent; the mass ratio of the aluminum chloride solid to the 3-aminopropyl trimethoxy silane is 1: 2;
(3) adding the PETG particles prepared in the step (1) into a mixed solvent of 1,1,2, 2-tetrachloroethane and xylene (volume ratio is 1: 1), mixing, adding an isocyanate type curing agent, heating to completely dissolve the isocyanate type curing agent, and then adding the isocyanate type curing agent into the modified aluminum chloride solution prepared in the step (2) to obtain a casting solution; and (3) dripping the casting film on the glass slide, placing the glass slide in a vacuum oven, and setting the temperature of the vacuum oven to be 120 ℃ to obtain the PETG aluminized composite film.
Example 3
A preparation method of a high-barrier PETG aluminized composite film comprises the following steps:
(1) 50 parts of PETG resin, 25 parts of polyvinyl alcohol, 20 parts of polycarbonate and 18 parts of styrene are put into an extruder, melted, blended and granulated to obtain PETG granules, and the PETG granules are dried until the moisture content is less than 1.5 per mill for later use; the extrusion capacity of the extruder is set to 1300kg/h, the extrusion temperature is 200 ℃, and the head temperature is 250 ℃;
(2) dissolving aluminum chloride in deionized water, performing ultrasonic dispersion, adding 3-aminopropyltrimethoxysilane under the stirring condition, and adjusting the pH value of the solution to be 2 by using hydrochloric acid to obtain a modified aluminum chloride solution; the mass concentration of aluminum ions in the modified aluminum chloride solution is 1.0 percent; the mass ratio of the aluminum chloride solid to the 3-aminopropyl trimethoxy silane is 1: 4;
(3) adding the PETG particles prepared in the step (1) into a mixed solvent of 1,1,2, 2-tetrachloroethane and xylene (volume ratio is 1: 1), mixing, adding an isocyanate type curing agent, heating to completely dissolve the isocyanate type curing agent, and then adding the isocyanate type curing agent into the modified aluminum chloride solution prepared in the step (2) to obtain a casting solution; and dripping the casting film on a glass slide, placing the glass slide in a vacuum oven, setting the temperature of the vacuum oven at 120 ℃, and drying until the solvent is completely volatilized to obtain the PETG aluminized composite film.
The method comprises the steps of cutting the membrane prepared in the examples 1-3 into an area of 60cm multiplied by 60cm, pressing the membrane into laminated glass, wherein the thickness of each piece of glass is 3.0mm, placing the laminated glass on an opening of a heat insulation box of 80cm multiplied by 80cm, placing a thermometer in the box, placing the box under a 150W infrared lamp for irradiating for 1 hour, and testing the air temperature in the box.
Table 1 results of performance tests of the composite films of examples 1 to 3.
Claims (10)
1. A preparation method of a high-barrier PETG aluminized composite film is characterized by comprising the following steps:
(1) putting the raw materials for preparing the PETG granules into an extruder, and carrying out melt blending granulation to obtain the PETG granules;
(2) dissolving aluminum chloride in deionized water, performing ultrasonic dispersion, adding a silane coupling agent under the stirring condition, and adjusting the pH of the solution to be acidic to obtain a modified aluminum chloride solution;
(3) adding the PETG particles prepared in the step (1) into a mixed solvent of 1,1,2, 2-tetrachloroethane and xylene, mixing, adding an isocyanate type curing agent, heating to completely dissolve the isocyanate type curing agent, and then adding the isocyanate type curing agent into the modified aluminum chloride solution prepared in the step (2) to obtain a casting solution; and dripping the casting film on a glass slide, and putting the glass slide in a vacuum oven until the solvent is completely volatilized to obtain the PETG aluminized composite film.
2. The preparation method of the high-barrier PETG aluminized composite film according to claim 1, wherein the PETG film is composed of the following components in parts by weight: 30-50 parts of PETG resin, 20-30 parts of polyvinyl alcohol, 10-20 parts of polycarbonate and 10-20 parts of styrene.
3. The preparation method of the high-barrier PETG aluminized composite film according to claim 1, wherein the PETG film is composed of the following components in parts by weight: 40-50 parts of PETG resin, 20-25 parts of polyvinyl alcohol, 15-20 parts of polycarbonate and 13-18 parts of styrene.
4. The preparation method of the high-barrier PETG aluminized composite film is characterized in that in the step (1), the extrusion capacity of an extruder is set to be 1300kg/h, the extrusion temperature is 200-300 ℃, the head temperature is 250 ℃, and the obtained pellets are dried until the moisture content is less than 1.5 per mill.
5. The preparation method of the high-barrier PETG aluminized composite film according to claim 1, wherein the temperature of the vacuum oven is 120-150 ℃.
6. The method for preparing the high-barrier PETG aluminized composite film according to claim 1, wherein the silane coupling agent is 3-aminopropyltrimethoxysilane or N, N-bis- (beta-hydroxyethyl) -gamma-aminopropyltriethoxysilane.
7. The preparation method of the high-barrier PETG aluminized composite film according to claim 1, wherein the mass concentration of aluminum ions in the modified aluminum chloride solution is 0.1% -1.0%.
8. The preparation method of the high-barrier PETG aluminized composite film according to claim 1, wherein in the step (2), the mass ratio of aluminum chloride to the silane coupling agent is 1: 2-1: 4; and adjusting the pH value of the solution to 2-4 by using hydrochloric acid.
9. The method for preparing the high-barrier PETG aluminized composite film according to claim 1, wherein the volume ratio of 1,1,2, 2-tetrachloroethane to xylene is 1: 1.
10. The high-barrier PETG aluminized composite film prepared by the preparation method of any one of claims 1-9.
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CN105435651A (en) * | 2015-12-22 | 2016-03-30 | 山东科技大学 | Method for preparing strong-hydrophilicity PET membrane |
CN105694089A (en) * | 2016-04-27 | 2016-06-22 | 山东科技大学 | Preparation method of super-hydrophilic PET membrane material |
CN108544826A (en) * | 2018-05-07 | 2018-09-18 | 安徽大学 | Montmorillonite-based high-barrier nano composite film and preparation method thereof |
CN109135607A (en) * | 2018-08-23 | 2019-01-04 | 天津博苑高新材料有限公司 | A kind of lamination fabrication Film laminated substrate and the manufacturing process of durability |
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2020
- 2020-10-27 CN CN202011162804.3A patent/CN112210102A/en not_active Withdrawn
Patent Citations (7)
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CN102284254A (en) * | 2011-06-10 | 2011-12-21 | 南京帝膜净水材料开发有限公司 | Method for manufacturing chlorine-resistant polyamide reverse osmosis composite film |
WO2015167235A1 (en) * | 2014-04-30 | 2015-11-05 | 코오롱인더스트리 주식회사 | Polyester film and method for manufacturing same |
CN104362207A (en) * | 2014-11-14 | 2015-02-18 | 无锡中洁能源技术有限公司 | High-resistance solar panel back membrane and preparation method thereof |
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