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Photochromic low-melting-point polyester master batch and preparation method thereof

A low-melting point polyester and photochromic technology, applied in the field of polyester, can solve the problems of poor reusability and light durability, easy loss of color-changing performance, poor color-changing effect, etc., to achieve good color-changing effect, low crystallinity, activity large space 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

[0007] Since the processing temperature of conventional polyester is above 260°C and the carboxyl-terminal content is greater than 20mol / t, the color-changing material is easy to lose its color-changing performance under high temperature and acidic conditions. The above patents have poor color-changing effect, poor stability, repeated use and light durability. Poor and other problems, so there is no batch product in the application

Method used

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  • Photochromic low-melting-point polyester master batch and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 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

[0035] 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 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 the po...

Embodiment 3

[0038] 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 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 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 po...

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Abstract

The invention discloses a photochromic low-melting-point polyester master batch and a preparation method thereof. The preparation 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 reaction under the action of a catalyst so as to prepare the low-carboxyl-terminated PBT or PET modified copolyester with the melting point range of 140-190 DEG C; and fullycrushing the low-melting-point polyester PET or PBT slices, uniformly mixing with a photochromic material, a heat stabilizer, a light stabilizer and an antioxidant according to a certain ratio in a high-speed mixer, carrying out melt blending by using a double-screw extruder, bracing, and carrying out underwater granulation to obtain the photochromic low-melting-point polyester master batch. The photochromic low-melting-point polyester master batch is good in color-changing effect, good in stability and good in illumination durability, and can be applied to engineering plastics, films, fiber products, 3D printing materials and the like.

Description

technical field [0001] The invention relates to the technical field of polyester, in particular to a photochromic low-melting polyester masterbatch and a preparation method thereof. Background technique [0002] With the development of science and technology and the improvement of people's living standards, the original application scope of textiles has already been broken through, and it tends to be functional and intelligent. At present, the development of smart textiles and their applications have attracted people's attention. Intelligent color-changing textiles refer to textiles whose color can change with changes in the external environment (such as light, temperature, etc.). There are photosensitive color-changing textiles and temperature-sensitive color-changing textiles. Change together, and once the light disappears or the temperature drops to the initial state, the color will return to the previous state, so its color is reversible, and it has a wide range of uses...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/183C08G63/60C08G63/85C08G63/86C08J3/22C08L67/02C08L67/00C08K5/523C08K5/521C08K5/134
CPCC08J3/226C08G63/183C08G63/60C08G63/85C08G63/866C08J2367/02C08J2367/00C08K5/1345
Inventor 李晶张建李庆男李仁海黄娟
Owner CHINA PETROLEUM & CHEM CORP
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