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A kind of unsaturated spiro ring orthocarbonate expansion monomer and its synthesis method and application

A technology of spiro-orthocarbonate and expansion monomer, which is applied in the fields of adhesive additives, non-polymer adhesive additives, organic chemistry, etc., and can solve problems such as being inferior to epoxy resin, reducing shrinkage, and limiting wide application. , to achieve the effect of improving adhesion, reducing internal stress, and reducing resin shrinkage

Active Publication Date: 2022-04-12
NICHE TECH KAISER SHANTOU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the general spiro ring orthocarbonate expansion monomer, because it does not contain other active functional groups, cannot react with vinyl monomers, silicone resins, etc., so its shrinkage reduction effect in other thermosetting resin systems is obviously not as good as that of ring ring Oxygen resin, which limits the further widespread application of expanded monomers

Method used

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  • A kind of unsaturated spiro ring orthocarbonate expansion monomer and its synthesis method and application
  • A kind of unsaturated spiro ring orthocarbonate expansion monomer and its synthesis method and application
  • A kind of unsaturated spiro ring orthocarbonate expansion monomer and its synthesis method and application

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Embodiment 1

[0031] In the present embodiment, the synthetic method of unsaturated spiro ring orthocarbonate expansion monomer comprises the following steps:

[0032] (1) Weigh 6,8-dihydroxy-1-nonene, di-n-butyltin oxide and toluene (6,8-dihydroxy-1-nonene 0.1mol, di-n-butyltin oxide 0.1mol, toluene 150ml), added to the reaction vessel and stirred, and reacted at 150±2°C for 12 hours or until anhydrous was formed (in this step (1), the reaction vessel was a three-necked flask placed in an oil bath, and 6, After adding 8-dihydroxy-1-nonene, di-n-butyltin oxide and toluene into the three-necked flask, install a water separator and a reflux condenser, install a calcium chloride drying tube on the reflux condenser, and then carry out the reaction) ;

[0033] This step reacts by reaction formula (I), and continuously removes the water that generates in the reaction process;

[0034]

[0035] (2) Cool the reaction liquid in the reaction vessel to room temperature, then add carbon disulfide ...

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Abstract

The invention provides an unsaturated spiro ring orthocarbonate expansion monomer, the synthesis method of which comprises the following steps: (1) weighing 6,8-dihydroxy-1-nonene, di-n-butyltin oxide and toluene, Add it into the reaction vessel and stir it, and react at 150±2°C; (2) Cool the reaction solution in the reaction vessel to room temperature, then add carbon disulfide dropwise to the reaction solution, and then heat the reaction solution to 110±2°C, Continue the reaction; (3) Cool the reaction liquid to room temperature, remove the toluene, wash, recrystallize, and dry in vacuum to obtain the unsaturated spiro ring orthocarbonate expanded monomer. The above-mentioned unsaturated spiro orthocarbonate expansion monomer can be used as the anti-curing shrinkage component of the silicone resin encapsulation material. The unsaturated spiro ring orthocarbonate expansion monomer synthesized by the invention can not only expand through ring-opening polymerization, but also react with ethylenic monomers, acrylic resins or vinyl hydrogen-containing silicone resins, and can reduce resin shrinkage.

Description

technical field [0001] The invention relates to an expansion monomer, in particular to a synthesis method of an unsaturated spiro ring orthocarbonate expansion monomer and the application of the unsaturated spiro ring orthocarbonate expansion monomer in the preparation of silicone resin encapsulation materials. Background technique [0002] Thermosetting resins will inevitably shrink in volume during the curing process, resulting in shrinkage stress and becoming a potential destructive factor, which will lead to a sharp drop in material strength, or even cracking of the material; or lead to deterioration of the performance of electronic or optical components, parameters Drift; or cause the glued interface to be more susceptible to environmental factors such as water and acid. The causes of curing shrinkage include the overflow of solvent molecules, the elimination of small molecules, and the effect of Van der Waals force between monomer molecules into covalent bond after cur...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/10C09J183/07C09J183/05C09J11/06
CPCC07D493/10C09J183/04C09J11/06C08L2205/025C08L2205/03C08L83/04C08K5/1575
Inventor 周博轩冯兆丰罗永祥石逸武许喜銮
Owner NICHE TECH KAISER SHANTOU
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