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Preparation method of hyperbranched polyester graft modified sisal fiber cellulose microcrystal

A technology of hyperbranched polyester and cellulose microcrystals, applied in the field of polymer material modification, to achieve the effects of low price, wide source of raw materials, good interface compatibility and bonding strength

Active Publication Date: 2014-07-30
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above ideas have not been reported in the literature

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) Dissolve 1.5 grams of N, N-dicyclohexylcarbodiimide in 8 milliliters of DMF, 2 Under protection, it was gradually added dropwise to a 100 ml three-neck flask containing 4 g of malic acid and 8 ml of THF, stirred and reacted at 25°C for 12 hours, filtered to remove the off-white precipitate, and the filtrate was distilled to remove the solvent to obtain a light yellow oily viscous The product is a carboxyl-terminated hyperbranched polyester.

[0018] (2) in 100 milliliters of there-necked flasks, add 8 milliliters of DMF, 4 gram sisal cellulose microcrystals and 2 gram of step (1) the end carboxyl hyperbranched polyesters that make, in N 2 Stir and react at 30°C for 30 minutes under protection, then add 2 grams of N, N-diisopropylcarbodiimide and 0.2 grams of 4-dimethylaminopyridine, react at constant temperature for 12 hours, filter, and dry to obtain overrun Polyester grafting modified sisal cellulose microcrystals.

[0019] Get 0.26 grams of hyperbranched polyes...

Embodiment 2

[0022] (1) Dissolve 1.5 grams of N, N-dicyclohexylcarbodiimide in 8 milliliters of DMF, 2 Under protection, it was gradually added dropwise to a 100 ml three-neck flask containing 4 g of malic acid and 8 ml of THF, stirred and reacted at 25°C for 12 hours, filtered to remove the off-white precipitate, and the filtrate was distilled to remove the solvent to obtain a light yellow oily viscous The product is a carboxyl-terminated hyperbranched polyester.

[0023] (2) in 100 milliliters of there-necked flasks, add 10 milliliters of DMF, 5 gram sisal cellulose microcrystals and 4 gram of step (1) the end carboxyl hyperbranched polyesters that make, in N 2 Stir and react at 30°C for 30 minutes under protection, then add 4 grams of N, N-diisopropylcarbodiimide and 0.3 grams of 4-dimethylaminopyridine, react at constant temperature for 12 hours, filter, and dry to obtain the overrun Polyester grafting modified sisal cellulose microcrystals.

[0024] Get 0.78 grams of hyperbranched p...

Embodiment 3

[0027] (1) Dissolve 1.5 grams of N, N-dicyclohexylcarbodiimide in 8 milliliters of DMF, 2 Under protection, it was gradually added dropwise to a 100 ml three-neck flask containing 4 g of malic acid and 8 ml of THF, stirred and reacted at 25°C for 12 hours, filtered to remove the off-white precipitate, and the filtrate was distilled to remove the solvent to obtain a light yellow oily viscous The product is a carboxyl-terminated hyperbranched polyester.

[0028] (2) in 100 milliliters of there-necked flasks, add 10 milliliters of DMF, 6 gram sisal cellulose microcrystals and 4 gram step (1) the end carboxyl hyperbranched polyesters that make, in N 2 Stir and react at 35°C for 35 minutes under protection, then add 6 g of N, N-diisopropylcarbodiimide and 0.4 g of 4-dimethylaminopyridine, react at constant temperature for 12 hours, filter, and dry to obtain overrun Polyester grafting modified sisal cellulose microcrystals.

[0029] Get 1.3 grams of hyperbranched polyester grafted...

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Abstract

The invention discloses a preparation method of a hyperbranched polyester graft modified sisal fiber cellulose microcrystal, which comprises the following steps: dissolving N,N-dicyclohexylcarbodiimide in N,N-dimethylformamide, gradually dropwisely adding into a three-neck flask containing malic acid and tetrahydrofuran under the protection of N2, reacting at 30-40 DEG C for 12 hours while stirring, then filtering to remove grey-white precipitate, and distilling the filtrate to remove solvent, thus obtaining a light yellow oil-like sticky matter, namely carboxyl-terminated hyperbranched polyester; and adding N,N-dimethylformamide, a sisal fiber cellulose microcrystal and the prepared carboxyl-terminated hyperbranched polyester into the three-neck flask, reacting at 30-40 DEG C for 10-30 minutes under the protection of N2 while stirring, then adding N,N-diisopropylcarbodiimide and 4-dimethylaminopyridine, performing thermostatic reaction for 12 hours, filtering, and drying to obtain the hyperbranched polyester graft modified sisal fiber cellulose microcrystal. The method disclosed by the invention is wide in raw material sources, low in raw material price, less in pollution and simple in process; and the obtained product has favorable performance, and can obviously improve the comprehensive performance of a composite material.

Description

technical field [0001] The invention belongs to the technical field of polymer material modification, in particular to a method for preparing hyperbranched polyester graft modified sisal cellulose microcrystals. The prepared hyperbranched polyester graft-modified sisal cellulose microcrystals can be used for reinforcing and modifying thermosetting resins, thermoplastic resins, coatings, etc., and can significantly improve the mechanical properties and thermal properties of composite materials. Background technique [0002] In recent years, with the enhancement of people's awareness of environmental protection, the awareness of ecological and resource protection has also been continuously improved. The use of various fibers to modify polymer matrix composites has become a hot spot in material science research. Because natural fibers have the characteristics of wide source, low density, non-toxic and harmless, high strength and modulus, easy surface modification and low price...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G81/00C08G63/06C08L63/00C08J5/06
Inventor 陆绍荣肖仙娥徐旭虞锦洪祁博曾岑
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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