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Poly-2,5-furandicarboxylate-2,3-butylene glycol ester and its preparation method

A technology of furandicarboxylic acid and butanediol ester, which is applied in the field of polyester, can solve the problems of not completely based on renewable resources, environmental friendliness needs to be improved, etc., and achieves the effects of easy operation and wide sources

Active Publication Date: 2016-03-30
芜湖万隆新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, in the prior art, there are studies on the preparation of polyester or copolyester by using 2,5-furandicarboxylic acid or its derivatives and straight-chain aliphatic alcohol diols and cyclic diols as raw materials. However, in these studies The raw materials are not entirely based on renewable resources, and the environmental friendliness still needs to be improved

Method used

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  • Poly-2,5-furandicarboxylate-2,3-butylene glycol ester and its preparation method
  • Poly-2,5-furandicarboxylate-2,3-butylene glycol ester and its preparation method
  • Poly-2,5-furandicarboxylate-2,3-butylene glycol ester and its preparation method

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[0036] The present invention also provides a preparation method of poly-2,5-furandicarboxylate-2,3-butylene glycol, comprising the following steps:

[0037] a) reacting 2,5-furandicarboxylic acid and 2,3-butanediol under the action of a tetravalent titanium compound catalyst to obtain an intermediate product;

[0038] b) polycondensing the intermediate product under the condition of a pressure of 10Pa to 70Pa to obtain poly-2,5-furandicarboxylate-2,3-butylene glycol;

[0039] Described tetravalent titanium compound catalyst comprises:

[0040] Mesoporous silica modified by an organic modifier, the organic modifier is a titanate coupling agent or a silane coupling agent;

[0041] A tetravalent titanium compound supported on the mesoporous silica.

[0042] In the embodiment of the present invention, 2,5-furandicarboxylic acid, 2,3-butanediol and a tetravalent titanium compound catalyst are firstly mixed, and then reacted to obtain an intermediate product.

[0043] The inventi...

Embodiment 1

[0064] In the reactor, add 0.6g specific surface area is 850m 2 / g of dry SBA-15, 0.06g of isopropyl tris (dioctyl pyrophosphoryl) titanate organic modifier and 300mL of toluene, nitrogen with a flow rate of 0.5L / min as protective gas, dispersed by ultrasonic After 30 minutes, continue to stir and heat to 90°C for reaction. After 5 hours of reaction, the obtained reaction product dispersion liquid is rotary evaporated, and the solid obtained after rotary evaporation is washed and filtered to obtain organic modifier-modified SBA- 15;

[0065] In the loader, add 0.4g of SBA-15 modified by the organic modifier, 0.2g of tetrapropyl titanate and 200mL of toluene, pass through nitrogen as a protective gas, and after ultrasonic vibration for 30min, magnetically stir at 25°C After 48 hours, stop stirring and heating. After the reaction, excess tetrapropyl titanate was removed by suction filtration and washing, repeated several times, and then dried to obtain tetrapropyl titanate / SBA...

Embodiment 2

[0068] In the reactor, add 0.6g specific surface area is 1000m 2 / g dry MCM-41, 0.03g gamma aminopropyltrimethoxysilane organic modifier and 300mL toluene, nitrogen gas with a flow rate of 0.5L / min as protective gas, after ultrasonic dispersion for 30min, continue stirring and heating to The reaction was carried out at 90°C, and after 5 hours of reaction, the obtained reaction product dispersion liquid was rotated to evaporate, and the solid obtained after the rotary evaporation was washed and filtered to obtain MCM-41 modified by an organic modifier;

[0069] In the loader, add 0.4g of MCM-41 modified by the organic modifier, 0.4g of tetrabutyl titanate and 200mL of toluene, pass through nitrogen as a protective gas, and after ultrasonic vibration for 30min, magnetically stir at 25°C After 48 hours, stop stirring and heating. After the reaction, excess tetrabutyl titanate was removed by suction filtration and washing, repeated several times, and then dried to obtain tetrabut...

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Abstract

The invention provides poly furan-2,5-dicarboxylic acid-2,3-butanediol diacrylate and a preparation method thereof. The method comprises the following steps of reacting furan-2,5-dicarboxylic acid with 2,3-butanediol under the action of a tetravalent titanium compound catalyst, performing condensation polymerization on obtained intermediate products under the pressure of 10Pa-70Pa to obtain the product poly furan-2,5-dicarboxylic acid-2,3-butanediol diacrylate, wherein the tetravalent titanium compound catalyst comprises organic modifier-modified mesoporous silica and a tetravalent titanium compound which is loaded onto the mesoporous silica, wherein an organic modifier is a titanate coupling agent or a silane coupling agent. The product has at least one of first repeating unit shown by a formula (I), a second repeating unit shown by a formula (II) and a third repeating unit shown by a formula (III), and the intrinsic viscosity of the product is not lower than 0.5 deciliter per gram (0.5dL / g). Moreover, the preparation method is environmentally friendly and simple.

Description

technical field [0001] The invention relates to the technical field of polyester, in particular to a poly-2,5-furandicarboxylate-2,3-butylene glycol ester and a preparation method thereof. Background technique [0002] Polyester is a general term for polymers obtained by polycondensation of polyols and polyacids, including polyethylene terephthalate (PET), polybutylene terephthalate (PBT), polybutylene succinate Alcohol ester (PBS) and polyarylate, etc., have good mechanical properties and molding processing properties, and are widely used in the fields of fibers, films, resins and medical materials. [0003] With the improvement of people's living standards and the enhancement of environmental protection awareness, people pay more and more attention to resources and living environment. At present, almost all the raw materials used in the synthesis of polyester come from non-renewable petroleum resources. Therefore, the development is based on renewable resources, Environme...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/672
Inventor 周光远姜敏芦婷婷张强
Owner 芜湖万隆新材料有限公司
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