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Synthesis method of spiro orthoester-epoxy resin copolymer

A spirocyclic orthoester, epoxy resin technology, applied in the field of copolymer synthesis, can solve problems such as limited application and volume shrinkage

Inactive Publication Date: 2011-08-24
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Description
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Problems solved by technology

Epoxy resin is a widely used thermosetting polymer material, but due to its volume shrinkage (although small) during curing, its application in some special occasions is limited

Method used

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  • Synthesis method of spiro orthoester-epoxy resin copolymer
  • Synthesis method of spiro orthoester-epoxy resin copolymer
  • Synthesis method of spiro orthoester-epoxy resin copolymer

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Embodiment Construction

[0013] The present invention will be described in detail below with reference to the accompanying drawings.

[0014] The raw materials and reagents of the present invention are products of epoxy resin (E-54, E-44) Shenyang Chemical Factory; boron trifluoride monoethylamine (BF 3 -NH 2 Et, analytically pure) is a product of Tokyo Chemical Industry Co., Ltd., Japan, g-butyrolactone (chemically pure); boron trifluoride ether (analytically pure).

[0015] First carry out the synthesis of spiro ring ortho ester, the reaction equation sees figure 1 .

[0016] The synthesis steps: add 140ml of toluene and 25ml of g-butyrolactone into a three-neck flask; take 25g of E-54 and fully dissolve it in 45ml of toluene, put it into the dropping funnel; take the catalyst BF 3 ·OEt 2 Dissolve 0.66ml in 20ml of toluene and add in three times with an interval of 40min between each time. Use an ice-salt bath to cool down to about -12°C. After adding the first batch of catalysts, start adding...

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Abstract

The invention relates to a synthesis method of a spiro orthoester-epoxy resin copolymer, which comprises the following steps: synthesis of spiro orthoester: adding phenylmethane and gamma-butyrolactone into a three-neck flask, sufficiently dissolving E-54 in phenylmethane, pouring the reaction liquid into a separating funnel, washing out excessive gamma-butyrolactone, washing with deionized water to neutral, drying by adding anhydrous magnesium sulfate into the solution, filtering, and distilling under reduced pressure to remove phenylmethane, thereby obtaining the milky waxy spiro orthoester monomer; preparation of modified epoxy resin: taking the spiro orthoester, respectively adding to the epoxy resin E-44, adding mixed resin BF3.NH2Et, evenly mixing, and cooling to room temperature for later use; and evenly spreading the prepared modified epoxy resin between two potassium bromide salt flakes, and after the two potassium bromide salt flakes are fixed, curing by putting the two potassium bromide salt flakes into a baking oven which is preheated to 120 DEG C. The tensile strength and shear strength of the spiro orthoester-epoxy resin copolymer are on the rise, the rising trend of the shear strength is especially obvious, and thus, the mechanical properties of the modified epoxy resin matrix are enhanced.

Description

technical field [0001] The invention relates to a synthesis method of a copolymer, in particular to a synthesis method of a spirocyclic ortho ester and epoxy resin copolymer. Background technique [0002] Professor Bailey found that when spiro ring ortho ester monomers undergo double ring-opening polymerization under the action of a cationic initiator, the volume expands 〔1〕 , this phenomenon has aroused great interest of polymer materials scientists. Ordinary monomers and prepolymer resins are always accompanied by volume shrinkage during polymerization, especially the volume shrinkage caused by the further curing of thermosetting resins after gelation, which causes shrinkage stress inside the resin material, which is prone to stress concentration, which leads to One of the main reasons for the deterioration of the mechanical properties of materials and the reduction of service life. Often by adding some kind of filler to reduce the shrinkage, in order to achieve the purp...

Claims

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Application Information

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IPC IPC(8): C08G59/26C08G59/50
Inventor 王长松宁志高梁兵李安东刘大晨
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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