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Preparation method of polyfurandioctyl phthalate glycol ester

A technology of polyethylene furandicarboxylate and ethylene furandicarboxylate, which is applied in the field of bio-based polyester synthesis, can solve problems such as high molecular weight and color, and achieve improved product color, increased molecular weight, The effect of excellent mechanical properties

Active Publication Date: 2016-12-21
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] In summary, there are no patents and bibliographical reports of polyethylene furandicarboxylate with high molecular weight, good color and easy preparation method

Method used

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  • Preparation method of polyfurandioctyl phthalate glycol ester

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) Add dimethyl furandicarboxylate (0.1mol, 18.4g), ethylene glycol (0.25mol, 15.5g) and 1,8-diazabicycloundec-7-ene (0.1mmol, 20.7 mg), reacted at 170°C for 1h, 180°C for 1h, and 190°C for 2 hours to obtain the transesterification product;

[0042] (2) Under the conditions of 250° C. and 150 Pa, the melt polycondensation reaction was carried out for 5 hours to obtain polyethylene furandicarboxylate PEF1.

[0043] After testing, the intrinsic viscosity of PEF1 is 0.83dL / g; the absorbance at 400nm is 0.05.

Embodiment 2

[0045] (1) Add dimethyl furandicarboxylate (0.1mol, 18.4g), ethylene glycol (0.25mol, 15.5g) and 1,8-diazabicycloundec-7-ene to coordinate the supported catalyst ( 0.1mmol, 16.8mg), reacted at 170°C for 1h, 180°C for 1h, and 190°C for 1 hour to obtain the transesterified product;

[0046] (2) Under the conditions of 240° C. and 150 Pa, the melt polycondensation reaction was carried out for 3 hours to obtain polyethylene furandicarboxylate PEF2.

[0047] After testing, the intrinsic viscosity of PEF2 is 0.96dL / g; the absorbance at 400nm is 0.03.

[0048] The preparation of the 1,8-diazabicycloundec-7-ene coordination supported catalyst comprises the following steps:

[0049] (i) Mix 10ml of n-butyl titanate in 100ml of hydrochloric acid with a concentration of 1mol / L, stir for 5h to obtain TiO 2 Sol;

[0050] (ii) In the above TiO 2 Add 4.5g talcum powder and 10g 1,8-diazabicycloundec-7-ene to the sol, stir for 3 hours, filter and centrifuge to obtain a white precipitate, w...

Embodiment 3

[0053] (1) Add dimethyl furandicarboxylate (0.1mol, 18.4g), ethylene glycol (0.25mol, 15.5g) and polyvinylpyrrolidone with a supported catalyst (0.1mmol, 20.9mg), react at 170°C for 1h, React at 180°C for 1 hour, and react at 190°C for 0.5 hour to obtain the transesterified product;

[0054] (2) Under the conditions of 250° C. and 200 Pa, the melt polycondensation reaction was carried out for 2 hours to obtain polyethylene furandicarboxylate PEF4.

[0055] After testing, the intrinsic viscosity of PEF4 is 1.35dL / g; the absorbance at 400nm is 0.02; the mechanical properties of PEF4 are as follows figure 1 shown.

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Abstract

The invention discloses a preparation method of polyfuran dioctyl phthalate glycol ester. The preparation method comprises the following steps: (1) esterification or ester exchange reaction: adding furan dioctyl phthalate or furan dioctyl phthalate diester, ethylene and nitrogen-containing catalyst to a reactor, and reacting for 2-5 hours at 160-210 DEG C to obtain an esterification or ester exchange product; (2) polycondensation: reacting the esterification or ester exchange product in the conditions of pressure of less than or equal to 150Pa and temperature of 220-250 DEG C to prepare polyfuran dioctyl phthalate glycol ester. According to the invention, the efficient and high-selectivity nitrogen-containing catalyst is adopted, thus being favorable for improving the esterification or ester exchange rate, promoting polycondensation and improving molecular weight; and the prepared product is colorless or shallow in color, less in byproducts and good in structure regularity. According to the preparation method, only one nitrogen-containing catalyst is needed and is only added before reaction, adding of catalyst is not needed in the medium process, the process is very simple, the process is environmentally friendly, and realization of industrialization is facilitated.

Description

technical field [0001] The invention relates to the technical field of bio-based polyester synthesis, in particular to furandicarboxylic acid or furandicarboxylic acid diester and ethylene glycol under the catalysis of a nitrogen-containing catalyst to prepare polyfuran through esterification, transesterification and polycondensation Ethylene glycol dicarboxylate. Background technique [0002] In the polymer industry, polyesters represented by polyethylene terephthalate (PET) and polybutylene terephthalate (PBT) occupy a very important position, and the global annual output has exceeded 50 million tons . PET and other polyesters have excellent thermal and mechanical properties, and are widely used in synthetic fibers, food packaging films, engineering plastics and other fields. However, terephthalic acid, ethylene glycol, and butanediol, which are raw materials for these polyesters, all come from petroleum products, which is not conducive to the sustainable development of ...

Claims

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Application Information

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IPC IPC(8): C08G63/18C08G63/87
CPCC08G63/18C08G63/87
Inventor 吴佳萍吴林波
Owner ZHEJIANG UNIV
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