Preparation method of polyester for environment-friendly antimony-free film

An environmentally friendly, polyester technology, which is applied in the field of polyester film preparation using liquid titanium catalysts and a certain amount of additives, can solve the problem of inability to use titanium catalysts, unstable process conditions and parameters, and unqualified performance. problem, to achieve the effect of improved performance, simple modulation method, and improved L value

Inactive Publication Date: 2014-02-05
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The technical problem to be solved in the present invention is to disclose a method for preparing an environment-friendly polyester for antimony-free membranes, especially a method for preparing polyester for membranes using a liquid titanium catalyst and a certain amount of additives, in order to overcome the existing The following defects exist in the existing technology: due to the existing polyester production equipment, especially the equipment with large production capacity, titanium-based catalysts cannot be used. The solid content of diol is not suitable for device preparation; or the polyester for film that cannot obtain qualified performance by using a titanium-based catalyst, for example, the hue b value of the synthesized PET slice is above 7.0, and the slice is yellowish and cannot be used for drawing. membrane

Method used

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  • Preparation method of polyester for environment-friendly antimony-free film

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] (A) A 2L stainless steel reactor was used to synthesize PET slices for membranes. Mix 500g terephthalic acid (PTA) and 260g ethylene glycol (EG) evenly, add liquid titanium catalyst TY-1, 4×10 -6 (Based on the content of the atomic mass of titanium in the total weight of the polyester produced) It can also be based on the output of theoretical products or the input amount of raw materials. The esterification reaction was carried out at 220°C under a pressure of 0.1 MPa, and the reaction time was 4 hours;

[0040] (B) After the end of the esterification reaction, start vacuuming for pre-condensation reaction, the reaction temperature is 240°C, the reaction pressure is an absolute pressure of 101kPa and gradually decreases to 600Pa, and the reaction time is 0.5 hours

[0041] (C) The final polycondensation reaction was carried out at 270°C and a pressure of 50 Pa. After 120 minutes of reaction time, polyester chips with an intrinsic viscosity of 0.670, an L value of 85, an...

Embodiment 2

[0043] (A) A 2L stainless steel reactor was used to synthesize PET slices for membranes. Mix 500g PTA and 260g EG evenly, add titanium catalyst TY-1, 15×10 -6 (Based on the content of titanium atomic mass in the total weight of the polyester produced), no other additives are added. The esterification reaction was carried out at 270°C under a pressure of 0.3 MPa, and the reaction time was 1 hour;

[0044] (B) After the esterification reaction is finished, start vacuuming to carry out the pre-condensation reaction, the reaction temperature is 270 ° C, the reaction pressure is an absolute pressure of 101kPa and gradually drops to 600Pa, and the time is 1 hour;

[0045] (C) The final polycondensation reaction was carried out at 280°C and a pressure of 100 Pa. After a reaction time of 60 minutes, polyester chips with an intrinsic viscosity of 0.672, an L value of 86, and a b value of 3.5 were obtained.

Embodiment 3

[0047] (A) A 2L stainless steel reactor was used to synthesize PET slices for membranes. Mix 500g of PTA and 260g of EG evenly, carry out esterification reaction at 250°C and a pressure of 0.2MPa, and the reaction time is 2.5 hours;

[0048] (B) After the esterification reaction, add titanium catalyst 7×10 -6 (Based on the content of the titanium atomic mass in the total weight of the polyester produced), add the auxiliary agent silicon dioxide 3000×10 -6 , Magnesium acetate 3000×10 -6 , (according to the content in the total weight of the polyester produced), after stirring evenly, start vacuuming to carry out the pre-condensation reaction, the pre-condensation reaction temperature is 270 ° C, the reaction pressure is an absolute pressure of 101kPa gradually reduced to 600Pa, time for 45 minutes;

[0049] (C) The final polycondensation reaction was carried out at 275°C and a pressure of 70 Pa. After a reaction time of 105 minutes, polyester chips with an intrinsic viscosit...

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Abstract

The invention relates to a preparation method of polyester for an environment-friendly antimony-free film. The method comprises the following steps of (A) adopting terephthalic acid and ethylene glycol as basic raw materials to be made into slurry, adding the slurry into a reactor to have esterification reaction for 1h to 4h under the condition that the temperature is 220DEG C to 260DEG and the pressure is 0.1MPa to 0.3MPa, and obtaining an esterification product; (B) carrying out the pre-polycondensation reaction for 0.5h to 1.0h to obtain a pre-polymer under the condition that the reaction temperature is 240DEG C to 270DEG C and the pressure is gradually reduced from the absolute pressure of 101kPa to 600Pa; (C) carrying out the final polycondensation reaction for the prepolymer obtained in the step (B) for 1h to 2h to obtain a polyester product under the condition that the temperature is 270DEG C to 290DEG C and the absolute pressure is 150Pa to 50Pa. The liquid titanium catalyst and accessory ingredients of a given quantity can be added into the reaction system before or after the esterification reaction. The synthesized polyester does not contain precious metal such as antimony and is qualified in properties and suitable for producing a two-directional stretching film.

Description

technical field [0001] The invention relates to a method for preparing an environment-friendly antimony-free polyester for membranes, in particular to a method for preparing polyester for membranes by using a liquid titanium series catalyst and a certain amount of additives. Background technique [0002] BOPET biaxially oriented polyester film, that is, a biaxially oriented film made of polyester (PET), has the characteristics of high strength, good rigidity, transparency, and high gloss; it is odorless, colorless, tasteless, and outstanding toughness. , the tensile strength is 3 times that of PC film and nylon film, and the impact strength is 3 to 5 times that of biaxially oriented polypropylene (BOPP) film. It has good wear resistance, folding resistance, pinhole resistance and resistance Tear resistance, small heat shrinkage; good antistatic property, easy for vacuum aluminum plating; good heat resistance, cooking resistance, low temperature freezing resistance, good oil ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/183C08G63/78C08G63/85C08L67/02
Inventor 臧国强徐振发郭灵通冯志强李少山马颖涛朱燕刘建忠杨力芳曲建姚树盛
Owner CHINA PETROLEUM & CHEM CORP
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