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Unsaturated spiro orthocarbonate expanding monomer as well as synthesis method and application thereof

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

Active Publication Date: 2021-05-25
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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  • Unsaturated spiro orthocarbonate expanding monomer as well as synthesis method and application thereof
  • Unsaturated spiro orthocarbonate expanding monomer as well as synthesis method and application thereof
  • Unsaturated spiro orthocarbonate expanding monomer as well as synthesis method and application thereof

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Embodiment 1

[0032] In the present embodiment, the synthetic method of unsaturated spiro ring orthocarbonate expansion monomer comprises the following steps:

[0033] (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) ;

[0034] This step reacts by reaction formula (I), and continuously removes the water that generates in the reaction process;

[0035]

[0036] (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 orthocarbonate expanding monomer. The synthesis method of the unsaturated spiro orthocarbonate expanding monomer comprises the steps of (1) weighing 6, 8-dihydroxy-1-nonene, di-n-butyltin oxide and toluene, adding into a reaction container, stirring, and reacting at the temperature of 150+ / -2 DEG C; (2) cooling the reaction liquid in the reaction container to room temperature, dropwise adding carbon disulfide into the reaction liquid, heating the reaction liquid to the temperature of 110+ / -2 DEG C, and continuing the reaction; and (3) cooling the reaction liquid to room temperature, removing toluene in the reaction liquid, washing, recrystallizing, and drying in vacuum to obtain the unsaturated spiro orthocarbonate expansion monomer. The unsaturated spiro orthocarbonate expanding monomer can be used as an anti-curing shrinkage component of an organic silicon resin packaging material. The unsaturated spiro orthocarbonate expanding monomer synthesized by the invention not only can expand through ring-opening polymerization, but also can react with an alkene monomer, acrylic resin or vinyl hydrogen-containing silicon resin, so that the shrinkage rate of the resin can be reduced.

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 Applications(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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