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Thermochromic low-melting-point polyester film and preparation method thereof

A low-melting polyester, thermochromic technology, applied in the field of polyester, can solve the problems such as the processing temperature of color-changing materials should not exceed 230 ° C, the thermal stability of thermochromic materials is poor, and the space for the activity of color-changing functional groups is limited, so as to achieve bright colors. , add interest and fashion, good color effect

Active Publication Date: 2020-05-05
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the processing temperature of conventional PBT polyester is above 260°C, the processing temperature of conventional PET polyester is above 280°C, and the thermal stability of thermochromic materials is poor. It will lose the color changing function, so the processing temperature of the color changing material should not exceed 230°C
At the same time, organic color-changing materials have poor acid resistance, and the content of carboxyl-terminal groups in polyester exceeds 20mol / t. The active ingredients of organic thermochromic materials will chemically react with the carboxyl-terminal groups in polyester, and the color-changing effect is very poor.
In addition, due to the high crystallinity of PBT and PET polyesters, there are more hard segments, which limits the activity space of the color-changing functional groups in the masterbatch.

Method used

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  • Thermochromic low-melting-point polyester film and preparation method thereof
  • Thermochromic low-melting-point polyester film and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] In a 20L polymerization reactor, successively add 3500 grams of terephthalic acid, 162 grams of adipic acid, 3915 grams of 1,4-butanediol, and adipic acid-based polyester diol with a molecular weight of 500 (Hua Da Chemical Group Co., Ltd. Company brand CMA-1044) 435 grams, tetrabutyl titanate 3.4 grams. Fill the reaction kettle with nitrogen to 0.1MPa, and then discharge it from the rectification column, repeat the replacement 3 times, set the temperature to heat, and carry out the esterification reaction at 180 ° C ~ 230 ° C under normal pressure conditions, esterification 3-4 hours , when the water output reaches 2000-2500mL, add 11.1 grams of cyclohexanol, react for 20 minutes, close the rectification column, open the vacuum system, gradually open the vacuum valve, and transition from low vacuum to high vacuum within 45 minutes. The internal absolute pressure is reduced to below 100Pa, and at the same time, the temperature inside the reactor is raised to 250°C~260°C...

Embodiment 2

[0030] In a 20L polymerization reactor, 3500 grams of terephthalic acid, 252.9 grams of succinic acid, 2131.5 grams of ethylene glycol, 468.5 grams of polycarbonate diol with a molecular weight of 1000, and 0.24 grams of antimony acetate were successively added. Fill the reaction kettle with nitrogen to 0.1MPa, and then discharge it from the rectification column, repeat the replacement 3 times, set the temperature to heat, and carry out the esterification reaction at 260 ° C ~ 280 ° C and a pressure of 0.2 MPa, esterification 2-2.5 Hours, when the water output reaches 1200-1400mL, release the pressure, add 20.6 grams of isoamyl alcohol, react at normal pressure for 20 minutes, close the rectification column, open the vacuum system, gradually open the vacuum valve, and transition from low vacuum to vacuum within 45 minutes High vacuum, the absolute pressure in the reactor is reduced to below 100Pa, at the same time, the temperature in the reactor is raised to 280 ℃ ~ 300 ℃, and ...

Embodiment 3

[0033] In a 20L polymerization reactor, add 3,000 grams of terephthalic acid, 596.9 grams of glutaric acid, 4,670.4 grams of 1,4-butanediol, 1,129.5 grams of polyε-caprolactone diol with a molecular weight of 500, tetra-titanate Butyl ester 4.2 g. Fill the reaction kettle with nitrogen to 0.1MPa, and then discharge it from the rectification column, repeat the replacement 3 times, set the temperature to heat, and carry out the esterification reaction at 180 ° C ~ 230 ° C under normal pressure conditions, esterification 3-4 hours , when the water output reaches 2000-2500mL, add 5.3 grams of n-heptanol, react for 20 minutes, close the rectification column, open the vacuum system, gradually open the vacuum valve, and transition from low vacuum to high vacuum within 45 minutes. The absolute pressure is lowered below 100Pa, and at the same time, the temperature in the reactor is raised to 250°C to 260°C, and the polymerization reaction is carried out under this condition. The polyme...

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Abstract

The invention discloses a thermochromic low-melting-point polyester film and a preparation method thereof, and belongs to the field of polyester. The method comprises the following steps: taking terephthalic acid, 1, 4-butanediol or ethylene glycol as raw materials, adding aliphatic dibasic acid, polyester diol and a monohydroxy end-capping reagent by adopting a direct esterification method, and carrying out esterification and polymerization reactions to prepare the PBT or PET modified copolyester, crushing PET or PBT slices, uniformly mixing the crushed PET or PBT slices with a thermochromicmaterial, a heat stabilizer and an antioxidant in a high-speed mixer, and carrying out melt blending and pelletizing by using a double-screw extruder to obtain thermochromic low-melting-point polyester master batch; and using the prepared thermochromic low-melting-point polyester master batch as an intermediate layer and low-melting-point polyester as an outer layer to prepare three layers of thethermochromic low-melting-point polyester film. The prepared thermochromic polyester film is low in modulus, good in hand feeling, low in crystallinity, good in thermal adhesiveness and good in colorchanging performance, and can be widely applied to the fields of automobiles, buildings, heat-seal packaging films and the like.

Description

technical field [0001] The invention relates to the technical field of polyester, in particular to a thermochromic low-melting polyester film and a preparation method thereof. Background technique [0002] Thermochromic film refers to a functional film product whose color changes reversibly when the temperature changes. With the development of science and technology, the development and application of thermochromic films have attracted more and more attention. Chinese patent CN201320559072.0 discloses a PET film with a color-changing function. Adding a color-changing powder to PET polyester chips enables the PET film to be photosensitive and temperature-sensitive. Since the processing temperature of conventional PBT polyester is above 260°C, the processing temperature of conventional PET polyester is above 280°C, and the thermal stability of thermochromic materials is poor. The discoloration function will be lost, so the processing temperature of the discoloration material...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B32B27/36B32B27/06B32B27/20
CPCB32B27/08B32B27/20B32B27/36
Inventor 张建李晶李庆男李仁海黄娟
Owner CHINA PETROLEUM & CHEM CORP
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