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Method for preparing modified polytrimethylene terephthalate

A technology of polytrimethylene terephthalate and trimethylene phthalate, which is applied in the field of polyester, can solve the problems of restricting the development of PTT and the high market price of PTT, and achieve the goal of increasing spinning speed, reducing crystallization speed and reducing production cost Effect

Inactive Publication Date: 2017-12-29
SINOPEC YIZHENG CHEM FIBER +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The excellent performance of PTT determines its broad prospects. However, compared with PET and PBT, the market price of PTT is relatively high, which limits the further development of PTT. This is due to the high price of propylene glycol, the raw material for producing PTT. The production cost of raw material propylene glycol must be reduced first

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 360 grams of propylene glycol, 4 grams of glycerin, 325 grams of terephthalic acid, and 0.310 grams of tetrabutyl titanate into a 2L reaction kettle. After that, gradually increase the temperature and transfer to the low vacuum stage. After the low vacuum time is about 45min, enter the high vacuum polycondensation stage (vacuum<100Pa), the polycondensation temperature is 240℃~250℃, the stirring power increase value reaches the rated value 40w, and the synthesized PTT intrinsic viscosity 0.901dL / g, carboxyl terminal 23mol / t, color value (L / a / b) 87.3 / -1.1 / 3.5. The temperature of melting and crystallization measured by DSC is about 152°C, and the enthalpy of melting and crystallization is 32J / g.

Embodiment 2

[0019] Add 327g of propylene glycol, 325g of terephthalic acid, 0.2g of pentaerythritol, 0.01g of cobalt acetate, and 0.370g of tetrabutyl titanate into a 2L reactor, heat up, and control the temperature of the esterification reaction at 220°C to 230°C. After the theoretical amount of water has been melted, gradually increase the temperature and enter the low vacuum stage. After the low vacuum time is about 45 minutes, enter the high vacuum polycondensation stage (vacuum <100Pa), the polycondensation temperature is 245°C-250°C, and the stirring power increase value reaches the rated value of 40w. The synthesized PTT has an intrinsic viscosity of 0.910dL / g, a terminal carboxyl group of 26mol / t, and a color value (L / a / b) of 85.4 / -1.1 / 1.3. According to DSC test, the melting crystallization temperature is about 153°C, and the melting crystallization enthalpy is 36J / g.

Embodiment 3

[0021] Add 387 grams of propylene glycol, 325 grams of terephthalic acid, 0.5 grams of 1,2,3-trimethylolpropane, 0.171 grams of tetrabutyl titanate, and the matting agent TiO in a 2L reactor. 2 1.2 grams (0.76% polyester weight), heating up, the esterification reaction temperature is controlled at 230 ° C ~ 245 ° C, when the esterification water reaches the theoretical amount, gradually increase the temperature and transfer to the low vacuum stage, after the low vacuum time is about 45 minutes, enter the In the stage of high vacuum polycondensation (vacuum<100Pa), the polycondensation temperature is 250℃~265℃, the increase value of stirring power reaches the rated value of 40w, the intrinsic viscosity of the synthesized PTT is 0.912dL / g, the terminal carboxyl group is 32mol / t, and the color value (L / a / b) 83.6 / -0.98 / 5.5. DSC test shows that the melting crystallization temperature is about 154°C, and the melting crystallization enthalpy is 37.9J / g.

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Abstract

The invention discloses a method for preparing modified polytrimethylene terephthalate. The method comprises the following steps: mixing terephthalic acid, propylene glycol, a titanate catalyst and a branching agent, and performing synthesis by adopting direct esterification, wherein a molar ratio of the propylene glycol to the terephthalic acid is 2.2-2.6, the branching agent is glycerin, pentaerythritol or 1,2,3-trimethylolpropane, and the addition amount accounts for 0.001-2% of the theoretical weight of the polytrimethylene terephthalate. According to the preparation method disclosed by the invention, the added branching agent is a multifunctional carbon compound, so the synthesized polytrimethylene terephthalate (PTT) contains molecular chains of a certain amount of cross-linking structures. Due to the cross-linking structure, the high polymer chain integrity is damaged, the crystallization property of PTT is reduced, the melt crystallization temperature of the improved PTT is lower than 155 DEG C, the melt crystallization enthalpy does not exceed 40J / g, the melt crystallization temperature and the melt crystallization enthalpy of the modified PTT are obviously reduced compared with the melt crystallization temperature of 178 DEG C and the melt crystallization enthalpy of 55J / g in the conventional PTT, the crystallization speed of the modified PTT is obviously reduced, the spinning speed of the PTT can be increased during spinning, and the aim of reducing the production cost of PTT fibers is achieved.

Description

technical field [0001] The invention relates to the polyester field, in particular to a preparation method of polytrimethylene terephthalate. Background technique [0002] Polytrimethylene terephthalate (PTT) is a new type of semi-crystalline thermoplastic polyester. Compared with polyethylene terephthalate (PET) and butylene terephthalate (PBT), it has It has a unique spiral structure and can produce good elasticity. It also has the softness of nylon, the bulkiness of acrylic fiber and the stain resistance of polyester. In addition, it has a better hand feeling than polyester and avoids the defect of acrylic fiber that is easy to wear and tear. , It has better color fastness than nylon. In short, PTT integrates the advantages of various synthetic fibers. Due to the excellent performance of PTT, it is widely used in clothing, industry, decoration and engineering plastics, especially in the carpet field as a strong competitor of nylon. [0003] Among the many applications o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/20D01F6/62
CPCC08G63/20D01F6/62
Inventor 戴志彬何胜君王金堂夏峰伟王余伟朱兴松
Owner SINOPEC YIZHENG CHEM FIBER
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