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Modified rosin-based hyperbranched polyester and preparation method and application thereof

A hyperbranched polyester and rosin-based technology, applied in the field of preparation of rosin-based hyperbranched polyester, can solve the problems of low terminal hydroxyl content of hyperbranched polyester, many steps of hyperbranched polyester, and affecting product color. The effect of simple treatment method, cheap solvent, and few synthesis steps

Active Publication Date: 2013-03-20
南昌市龙然实业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[Thermosetting Resins, 2010, 25(l): 40-47] synthesized hyperbranched polyester using maleopimaric acid and epichlorohydrin as monomers, but the end of the hyperbranched polyester obtained by this method The hydroxyl content is low, which is not conducive to the later modification and utilization, and the product contains chlorine, which affects the color of the product
[Thermosetting resins; 2011,26(5):16-20] used pentaerythritol as the polyester core to undergo esterification reaction with dimethylol propionic acid, and then reacted with maleopimaric anhydride to synthesize a compound rich in end groups. Hyperbranched polyester macromolecules, this method only uses maleopimaric acid as one of the monomers, not as the main body, and there are many steps to synthesize hyperbranched polyester, which is not easy to operate

Method used

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  • Modified rosin-based hyperbranched polyester and preparation method and application thereof
  • Modified rosin-based hyperbranched polyester and preparation method and application thereof
  • Modified rosin-based hyperbranched polyester and preparation method and application thereof

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preparation example Construction

[0037] A kind of preparation method of rosin-based hyperbranched polyester, under the protection of nitrogen, after dissolving maleopimaric acid with aprotic solvent, adding strong acid catalyst, inserting N 2In the reactor of the device and the reflux condenser, heat up to 90°C, gradually add a certain amount of glycidyl alcohol, raise the temperature to 110°C, react for 0.5h to 24h, continue the reaction under vacuum, when the acid value reaches the required value, continue to vacuum Continue the reaction under reduced pressure at a temperature of 0.1-100kPa for 0.5h-5h, finish the reaction, lower the temperature, precipitate in a precipitant, filter, separate, and dry to obtain hyperbranched polyester.

[0038] The aprotic solvent includes one of N-dimethylformamide, N,N-dimethylacetamide, dimethyl sulfoxide and ethyl acetate, or a mixture of any two or more of them.

[0039] The catalyst used is a strong acid catalyst including one of concentrated sulfuric acid, p-toluenes...

Embodiment 1

[0057] The preparation of embodiment 1 hyperbranched polyester

[0058] Dissolve 0.005mol maleopimaric acid (2.0g) in 10g N,N-dimethylformamide solution, raise the temperature to 90°C, add 0.02g catalyst p-toluenesulfonic acid, add 0.005mol glycidol (0.37 g) React for 5 hours under nitrogen protection conditions until the acid value is lower than 10mg / g, then continue to react for 2 hours under a vacuum of 100kPa, precipitate with a large amount of deionized water after cooling down, filter, wash, and vacuum dry to obtain White powdery solid product 1.8g, yield 76.9%, number average molecular weight M n 730, weight average molecular mass M w It is 760, the molecular mass distribution is 1.03, and the degree of branching is 0.23.

Embodiment 2

[0059] The preparation of embodiment 2 hyperbranched polyester

[0060] Dissolve 0.005mol maleopimaric acid (2.0g) in 10g N,N-dimethylformamide solution, heat up to 90°C, add 0.02g catalyst p-toluenesulfonic acid, add 0.01mol glycidyl alcohol ( 0.74g), filled with nitrogen for 7 hours until the acid value is lower than 10mg / g, then reacted for 2 hours under a vacuum of 100kPa, stopped the reaction, lowered the temperature, precipitated with a large amount of deionized water, filtered, washed and dried in vacuum Obtain white powdery solid product 1.9g, yield is 69%, number average molecular weight M n 2060, weight average molecular mass M w It is 2340, the molecular mass distribution is 1.13, and the degree of branching is 0.63.

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Abstract

The invention discloses a modified rosin-based hyperbranched polyester and a preparation method and application thereof. The preparation method comprises the following steps of: taking maleopimaric acid and glycidol as a monomer, reacting for a certain period of time to obtain an initial product under catalysis condtions, reprecipitating, filtering, separating and drying to obtain the hyperbranched polyester; and taking acrylic acid, acryloyl chloride and the like as modifiers, and carrying out a modification reaction in solvents of toluene, dichloromethane and the like so as to prepare the modified rosin-based hyperbranched polyester. The method is simple, expensive equipment and complex operation are not required, and the polymer contains lots of end vinyl groups, has high photocuring reactivity, is suitable for serving as a curing agent and a prepolymer of other photocuring function materials and is wide in prospect.

Description

technical field [0001] The invention relates to a method for preparing hyperbranched polyester, in particular to a method for preparing rosin-based hyperbranched polyester. Background technique [0002] Hyperbranched polymer is a new type of polymer developed in the past two decades. It is composed of continuous branched repeating units, generally through AB x The (x≥2) type polyfunctionality monomer is obtained by one-step polymerization reaction, the reaction process is simple, no careful purification is required, and the complicated preparation process is omitted. Hyperbranched polymers have a highly branched three-dimensional spherical structure, a large number of end groups, no entanglement between molecules, good solubility, low viscosity, and high chemical reactivity, making them suitable for coatings and resins. Agents, polymer materials have good application prospects. [0003] Rosin is an important biomass resource in my country. In rosin resin acids, abietic aci...

Claims

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Application Information

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IPC IPC(8): C08G83/00
Inventor 赵振东孙丽婷陈玉湘卢言菊毕良武李冬梅王婧古研
Owner 南昌市龙然实业有限公司
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