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Synthetic method of castor oil derivative based long-chain HBP (hyperbranched polyester) with low viscosity and good chain segment flexibility

A technology of castor oil derivatives and hyperbranched polyesters, applied in the directions of organic chemistry, thioether preparation, etc., achieves the effects of excellent chain segment flexibility, good application prospects, and excellent fluidity

Inactive Publication Date: 2019-06-21
ZHEJIANG FORESTRY UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to MR-based bio-based AB n The flexible aliphatic main chain in the monomer molecule is relatively long (9-10) and the internal plasticizing effect of the pendant side chain (Y.J. Xuetal. Polymer 2008, 49, 4248), so the branched polyester obtained by polycondensation is expected to overcome the current Reported Hyperbranched Polyester T g high disadvantage

Method used

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  • Synthetic method of castor oil derivative based long-chain HBP (hyperbranched polyester) with low viscosity and good chain segment flexibility
  • Synthetic method of castor oil derivative based long-chain HBP (hyperbranched polyester) with low viscosity and good chain segment flexibility
  • Synthetic method of castor oil derivative based long-chain HBP (hyperbranched polyester) with low viscosity and good chain segment flexibility

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Weigh 10g of ricinoleic acid methyl ester (0.024mmol) with a purity of 75%, 5.6g of mercaptoethanol (0.072mmol) and 0.06g of DMPA (0.00024mmol) and place them in a quartz container, then put them into a UV lamp In a sealed iron box, under the conditions of magnetic stirring and ultraviolet light, take out after light click reaction for 2 hours, add 20ml ethyl acetate to the quartz container, mix well, transfer to a separatory funnel, wash with deionized water for 3-5 After washing, take the upper ethyl acetate phase, add anhydrous magnesium sulfate to dry for 12 hours, filter, and remove the solvent by rotary evaporation to obtain AB 2 type monomer. Take 5gAB 2 type monomer, 0.08g Sb 2 o 3(0.00027mmol) was placed in a three-necked flask equipped with a mechanical stirring device, into which nitrogen was introduced, and the reaction was stirred at 70°C for 2h, followed by stirring at 130°C for 2h, and finally the temperature was raised to 170°C, and the reaction was c...

Embodiment 2

[0032] Weigh 10g of ricinoleic acid methyl ester (0.024mmol) with a purity of 75%, 5.6g of mercaptoethanol (0.072mmol) and 0.06g of DMPA (0.00024mmol) and place them in a quartz container, then put them into a UV lamp In a sealed iron box, under the conditions of magnetic stirring and ultraviolet light, take out after light click reaction for 1 hour, add 20ml of ethyl acetate to the quartz container, mix well, transfer to a separatory funnel, and wash with deionized water for 3-5 After washing, take the upper ethyl acetate phase, add anhydrous magnesium sulfate to dry for 12 hours, filter, and remove the solvent by rotary evaporation to obtain AB 2 type monomer. Take 5gAB 2 type monomer, 0.08g Sb 2 o 3 (0.00027mmol) was placed in a three-necked flask equipped with a mechanical stirring device, and nitrogen gas was passed into it, and the reaction was stirred at 80°C for 2h, followed by stirring at 120°C for 2h, and finally the temperature was raised to 165°C, and the reacti...

Embodiment 3

[0034] Weigh 10g of ricinoleic acid methyl ester (0.024mmol), 7.5g of mercaptoethanol (0.096mmol) and 0.3g of DMPA (0.0012mmol) respectively in a quartz container with a purity of 75%, then put it into a UV lamp In a sealed iron box, under the conditions of magnetic stirring and ultraviolet light, take out after light click reaction for 1 hour, add 20ml of ethyl acetate to the quartz container, mix well, transfer to a separatory funnel, and wash with deionized water for 3-5 After washing, take the upper ethyl acetate phase, add anhydrous magnesium sulfate to dry for 12 hours, filter, and remove the solvent by rotary evaporation to obtain AB 2 type monomer. Take 5g AB 2 type monomer, 0.08g Zn(OAc) 2 (0.0004mmol) was placed in a three-necked flask equipped with a mechanical stirring device, nitrogen gas was introduced therein, the reaction was stirred at 80°C for 2h, then stirred at 120°C for 3h, and finally the temperature was raised to 175°C, and the reaction was carried out...

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Abstract

The invention discloses a synthetic method of castor oil derivative based long-chain HBP (hyperbranched polyester) with low viscosity and good chain segment flexibility. Biodegradable ricinoleic acidor methyl ricinoleate which is sourced from natural renewable resources is used as a starting material instead of a non-biodegradable petroleum based chemical, an ABn self-polycondensation monomer issynthesized conveniently and efficiently by an environment-friendly solvent-free thiol-ene photo-click reaction, and novel bio-based HBP is obtained finally in a staged polymerization manner. Comparedwith the conventional petroleum based HBP, synthesized bio-based HBP not only has highly-branched molecular structure of general HBP, but also has the advantages of low glass transition temperature,good fluidity and the like due to the specific structural characteristics that a main chain of HBP has longer soft segments and contains a large quantity of C6 aliphatic alkyl hanging side chains.

Description

technical field [0001] The invention relates to a method for synthesizing castor oil derivative-based long-chain hyperbranched polyester with low viscosity and good segment flexibility. Background technique [0002] Hyperbranched Polyesters (HBP) is a polymer with an asymmetric, highly branched structure, a wide molecular weight distribution, and its degree of branching is mostly between 0.4 and 0.8. HBP not only shows the similar structure and properties of dendritic polymers, but also has the advantages of simple synthesis process and easy industrialization compared with dendritic polymers. With lower viscosity and higher reactivity, it can be widely used in chemical industry, electronics, machinery manufacturing and other fields. [0003] There are many synthetic methods for hyperbranched polymers, among which self-condensation reaction is a relatively common method for preparing long-chain hyperbranched polyesters. The self-condensation reaction is due to the AB n In ...

Claims

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Application Information

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IPC IPC(8): C08G63/688C08G63/78C07C319/18C07C323/52
Inventor 刘宏治单鹏嘉
Owner ZHEJIANG FORESTRY UNIVERSITY
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