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Preparation of hyperbranched polymer and hyperbranched epoxy resin

A technology of hyperbranched polymer and epoxy resin, which is applied in the field of preparation of hyperbranched polymer, can solve the problems of heat resistance decline, and achieve the effects of excellent heat resistance, low raw material cost and simple process

Active Publication Date: 2009-07-08
苏州海博特树脂科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The resin has been proven to greatly enhance the bisphenol A type epoxy resin (Journal of Applied Polymer Science, 2006, 101: 2504-2511; Polymer-Plastics Technology and Engineering, 2006, 45: 1005-1011), and the tensile strength and flexural strength There is an improvement of more than 20%, but the heat resistance has dropped by nearly 10%

Method used

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  • Preparation of hyperbranched polymer and hyperbranched epoxy resin
  • Preparation of hyperbranched polymer and hyperbranched epoxy resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Prepare according to the hyperbranched epoxy resin of the present embodiment through the following steps successively:

[0031] (1), synthetic hydroxyl end hyperbranched polymer: with 0.9mol phthalic acid, 0.9mol trimethylolpropane, 0.1mol trimethylol cyanurate, 1.5g p-toluenesulfonic acid (consumption is monomer 0.5% of the total mass), 500ml of xylene and 100ml of dimethylacetamide were added to a three-necked flask equipped with a water separator, a condenser, a thermometer and a stirrer, and the temperature was slowly raised to 170-180°C, and kept at this temperature After reacting for 6 hours, a hyperbranched polymer containing 12 mol terminal hydroxyl groups was obtained.

[0032] (2), Synthesis of hyperbranched epoxy resin: 0.1mol of the hyperbranched polymer containing 12mol terminal hydroxyl groups prepared above, 4.8mol of epichlorohydrin and 0.05mol of cetyltrimethylammonium bromide are added to the reactor In the process, keep the reaction at 100°C for 2 ho...

Embodiment 2

[0034] Prepare according to the hyperbranched epoxy resin of the present embodiment through the following steps successively:

[0035] (1), synthetic carboxyl-terminated hyperbranched polymer: the consumption of 0.9mol phthalic anhydride, 0.12mol phthalic acid, 0.9mol diethanolamine, 0.1mol triamine methyl cyanurate, p-toluenesulfonic acid is the amount of monomer Add 0.8%, 800ml of xylene into a three-necked flask equipped with a water separator, a condenser, a thermometer and an agitator, slowly raise the temperature to 160-170°C, and keep the reaction at this temperature for 8 hours to obtain a hyperbranch containing 12mol terminal carboxyl groups. chemical polymer.

[0036] (2), synthetic hyperbranched epoxy resin: 0.1mol hyperbranched polymer prepared in step (1), 12mol epichlorohydrin and 0.12mol cetyltrimethylammonium bromide, under the condition of 110 ℃ After 6 hours of reaction, excess epichlorohydrin was removed in vacuo. Then drop to room temperature, add enough ...

Embodiment 3

[0038] Prepare according to the hyperbranched epoxy resin of the present embodiment through the following steps successively:

[0039] (1), the hyperbranched polymer of synthetic terminal hydroxyl: the consumption of 0.42mol trimellitic anhydride, 0.82mol ethylene glycol, 0.02mol trimethylol cyanurate, sulfuric acid is 0.5% of monomer, xylene 400ml, toluene Add 300ml and 100ml of dimethylformamide into a three-necked flask equipped with a water separator, condenser, thermometer and stirrer, slowly raise the temperature and react at 150-160°C for 10 hours to obtain a hyperbranched polymer.

[0040](2), synthetic hyperbranched epoxy resin: the hyperbranched polymer that 0.05mol step (1) makes, 10mol epichlorohydrin and 0.08mol concentration are 5% sodium hydroxide aqueous solution, under the condition of 60 ℃ After 10 hours of reaction, excess epichlorohydrin was removed in vacuo. Then lower it to room temperature, add enough ethanol to dissolve it fully under stirring conditi...

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Abstract

The invention relates to a preparation method for a hyperbranched epoxy resin. The preparation method comprises the following steps: (1) preparing a hyperbranched polymer with a functional end group; (2) carrying out the reaction of the hyperbranched polymer and chloroepoxy propane under the action of a ring opening catalyst to obtain an addition product; and (3) carrying out the ring closing reaction of the obtained addition product in an organic solvent and under the reaction of a basic catalyst to generate the hyperbranched epoxy resin, wherein the hyperbranched polymer is prepared under the action of the catalyst through the reaction of a first monomer and a second. Polybasic amine, polyol or the mixture thereof is taken as the first monomer; polyatomic acid, anhydride or the mixture thereof is taken as the second monomer; the dosage mol ratio of the first monomer to the second monomer is 1:0.3 to 2.5; and the first monomer at least comprises a heat resistant six-membered compound which is more than or equal to 1 percent of the total mol number of the first monomer. The prepared hyperbranched epoxy resin has low viscosity, high heat resistance, and the reinforcing and plasticizing functions for a common epoxy resin. The hyperbranched epoxy resin can be widely applied to the fields of electronic packaging, functional adhesives, and the like.

Description

technical field [0001] The invention belongs to the technical field of polymer material preparation, in particular to a preparation method of a hyperbranched polymer. Background technique [0002] Epoxy resin has the advantages of good mechanical and electrical properties, low shrinkage, easy processing and low price, and is widely used in adhesives, coatings, and advanced composite materials. However, due to its high crosslinking density and structural characteristics of benzene ring skeleton after curing, epoxy resin has poor impact resistance and insufficient toughness. [0003] In the prior art, the toughening methods of epoxy resin mainly include core-shell polymer toughening, IPN toughening, thermotropic liquid crystal polymer toughening, rubber-like elastomer toughening, nanoparticle toughening, and the like. However, these toughening methods will cause a significant decrease in the tensile strength and bending strength of the resin while improving the toughness of t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/28C08G63/12C08G59/20C08G59/68
Inventor 张道洪施文磊周继亮张春琪李廷成吕康乐徐晓风
Owner 苏州海博特树脂科技有限公司
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