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A kind of graft with itaconic acid as skeleton and preparation method thereof

A technology of graft and itaconic acid, which is applied in the field of bio-based and biodegradable materials, can solve problems such as easy surface migration, easy phase separation, and limited compatibility improvement

Active Publication Date: 2021-01-15
重庆虹彩盈田新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, when blending and filling, phase separation is very easy to occur, which deteriorates the performance of the product
The use of coupling agents and surfactants helps to improve compatibility to a certain extent, but such additives have low molecular weight and are prone to surface migration, so they are not suitable for use with food
Utilizing the hydroxyl groups contained in natural polymers to carry out etherification and esterification has been widely used in the field of modified starch, but such small molecule modification is beneficial to reduce hydrophilicity and improve thermoplastic processing, but has limited improvement in compatibility.

Method used

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  • A kind of graft with itaconic acid as skeleton and preparation method thereof
  • A kind of graft with itaconic acid as skeleton and preparation method thereof
  • A kind of graft with itaconic acid as skeleton and preparation method thereof

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Experimental program
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preparation example Construction

[0069] A preferred preparation method of the present invention is as follows, comprising steps:

[0070] (1) Monomethyl ester of itaconic acid. Itaconic acid, acid chloride reagent and dry methanol are mixed and heated to reflux state, after 30min-2h, cooled to room temperature. The crude product was recrystallized with a mixed solvent of petroleum ether to obtain product I (monomethyl β-itaconate).

[0071]

[0072] (2) Orthogonal protection of β-monomethyl itaconate. β-monomethyl itaconate reacts with di-tert-butyl pyrocarbonate (BOC2O) to protect the carboxyl group at the α position in the base 4-DMAT. The crude product was recrystallized from petroleum ether to obtain product II.

[0073]

[0074] (3) Demethylation of the product II in step (2). with MeOH:H 2 O=2:1, NaOH (2eq), heat to reflux for 1-4h, spin dry the solvent, extract, adjust the pH, extract with chloroform or dichloromethane, spin dry the solvent to obtain the demethylated product III.

[0075] ...

Embodiment 1

[0100] Add 0.10 mol of itaconic acid, 0.11 mol of dried methanol, and 60 mL of benzoyl chloride into a flask equipped with a reflux condenser and a sodium hydroxide solution gas absorption device. Heat the reaction liquid to reflux, slowly add benzoyl chloride dropwise, remove the heat when the hydrogen chloride gas is no longer discharged, cool to room temperature, remove the solvent by rotary evaporation and then distill under reduced pressure, collect 80-83°C fractions under 11mmHg pressure to obtain Product I (β-monomethyl itaconate).

Embodiment 2

[0102] Boc protection of β-monomethyl itaconate. 0.1 mol of β-monomethyl itaconate was dissolved in 50 mL of 4-DMAP as a solvent, and reacted with 0.06 mol of di-tert-butyl pyrocarbonate (BOC2O) under reflux for 3 hours to protect the carboxyl group at the α position. The crude product was recrystallized with petroleum ether, and the product II was obtained after drying.

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Abstract

The invention provides a graft taking itaconic acid as a framework and a preparation method thereof, and in particular, provides a high molecule graft combined with biomass nanocrystallines, poly alpha-hydroxyl acid chain segment and polyester chain segment by taking biological and degradable itaconic acid as the framework, and the graft is as shown in a formula (I). The graft provided by the invention can be used for meeting application demands in many fields such as packaging materials and films. Products prepared by the graft have excellent performances such as low cost, environment friendliness, degradability, high mechanical strength and the like. The formula is as shown in the description.

Description

technical field [0001] The invention belongs to the field of bio-based and biodegradable materials, and in particular relates to a graft of polysaccharide nanomaterials containing two different polyester structures with bio-based itaconic acid as a skeleton and a preparation method thereof. Background technique [0002] At present, the biodegradable polyesters that have been industrialized at home and abroad mainly include: polylactic acid (PLA), polyhydroxy fatty acid (PHA), polypropylene carbonate (PPC), polybutylene succinate (PBS), Polybutylene adipate / terephthalate (PBAT), polycaprolactone (PCL), etc. Various resin raw materials have their own characteristics in terms of price, physical and mechanical properties, processing performance and application fields. For example: PLA has high strength, elongation at break, poor impact resistance, and low heat distortion temperature, but its processing performance is superior, and it is suitable for processing methods such as i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/91C08G63/08C08G81/00C08L87/00C08L3/02C08L1/04
CPCC08G63/08C08G63/912C08G81/00C08L87/005C08L2201/06C08L3/02C08L1/04
Inventor 不公告发明人
Owner 重庆虹彩盈田新材料科技有限公司