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Preparation method for rosin-based hyperbranched polyester and application of rosin-based hyperbranched polyester in epoxy resin

A hyperbranched polyester and rosin-based technology, which is 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, unfavorable modification and utilization, etc., to achieve Inexpensive solvents, fewer synthesis steps, and easy development and utilization

Active Publication Date: 2014-01-22
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[Thermosetting Resins, 2010,25(1):40-47] used maleopimaric acid and epichlorohydrin as monomers to synthesize hyperbranched polyester, 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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  • Preparation method for rosin-based hyperbranched polyester and application of rosin-based hyperbranched polyester in epoxy resin
  • Preparation method for rosin-based hyperbranched polyester and application of rosin-based hyperbranched polyester in epoxy resin
  • Preparation method for rosin-based hyperbranched polyester and application of rosin-based hyperbranched polyester in epoxy resin

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preparation example Construction

[0020] 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 2 In the reactor of the device and the reflux condenser, heat up to 90°C, gradually add a certain amount of glycidol, raise the temperature to 110°C, react for 0.5h to 24h, vacuumize and continue the reaction, 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. Its chemical reaction formula is as follows:

[0021]

[0022] The aprotic solvent includes one of N-methylformamide, N,N-methylacetamide, dimethyl sulfoxide, and ethyl acetate, or a mixture of any two or more of them.

[0023] The catalyst used is a strong acid catalyst includ...

Embodiment 1

[0042] 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 the condition of nitrogen protection, follow up and check that the acid value is below 10mg / g, then continue to react for 2 hours under a vacuum of 100kPa and cool down, then precipitate with a large amount of deionized water, 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 weight M wIt is 755, the molecular weight distribution is 1.03, and the degree of branching is 0.23.

Embodiment 2

[0044] 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 0.01mol glycidol (0.74 g) React with nitrogen gas for 7 hours, follow up and check that the acid value is below 10mg / g, then react for 2 hours under a vacuum of 100kPa, stop the reaction, cool down, precipitate with a large amount of deionized water, filter, wash, and vacuum dry Obtain white powdery solid product 1.9g, yield is 69%, number average molecular weight M n 2064, weight average molecular weight M w It is 2343, the molecular weight distribution is 1.13, and the branching degree is 0.63.

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Abstract

The invention discloses a preparation method for rosin-based hyperbranched polyester and application of the rosin-based hyperbranched polyester to epoxy resin. The method comprises the following steps of: under the protection of nitrogen, reacting maleopimaric acid with a glycidol monomer in a molar ratio of (0.05-10):1 in an aprotic solvent at the temperature of 50 to 150 DEG C for 0.5 to 24 hours; adding a strong acid catalyst into the aprotic solvent, tracking and checking until an acid value is less than or equal to 10mg / g, reducing pressure at the vacuum degree of 0.1 to 100kPa, and continuously reacting for 0.5 to 5 hours to obtain an initial product; and precipitating, filtering, separating, and performing vacuum drying to obtain the rosin-based hyperbranched polyester. The method is simple, expensive equipment and complicated operation are not needed, and the obtained polymer contains a large number of end groups, can be dissolved in various organic solvents, and can be directly applied to the epoxy resin.

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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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00C08G59/62
Inventor 赵振东孙丽婷陈玉湘毕良武李冬梅卢言菊王婧古研
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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