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Phosphorus-containing spiro-compound and preparation method thereof

A technology of spiro compounds and compounds, applied in the field of phosphorus-containing spiro compounds and their preparation, can solve problems such as performance failure, composite material cracking, and strength decline, and achieve high product purity and yield, and production process conditions Simple, easy post-processing effect

Inactive Publication Date: 2013-11-27
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is a common problem in the developed polymer materials: the performance of its practical application is far from its theoretical performance.
The existence of this residual stress also makes the material prone to aging, which affects the service life of the material
[0003] The widely used epoxy resin will inevitably produce a certain residual stress due to volume shrinkage when it is cured. The residual stress in the resin is a potential destructive factor, which makes the interface between the resin and the fiber or the adhesive joint in the absence of external load. It is subject to considerable stress, resulting in a decrease in strength, and even cracking of the composite material, dimensional instability or degumming of the glued joints, etc.

Method used

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  • Phosphorus-containing spiro-compound and preparation method thereof
  • Phosphorus-containing spiro-compound and preparation method thereof
  • Phosphorus-containing spiro-compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 0.1 mol of phosphorus-containing glycol and 0.1 mol of di-n-butyltin oxide into a 500ml three-necked flask equipped with a water separator, reflux condenser, thermometer and magnet, add 200ml of toluene, and react at 130°C for 8 hours. After the reaction, cool down to room temperature, and slowly add 0.05mol of CS 2 , then reacted at 100°C for 12 hours, evaporated the solvent under reduced pressure, washed the viscous liquid at the bottom several times with n-hexane, recrystallized with toluene, filtered with suction, and dried to obtain 53.5 g of light yellow crystals with a yield of 75.7%.

Embodiment 2

[0023] Add 0.1 mol of phosphorus-containing glycol and 0.1 mol of di-n-butyltin oxide into a 500ml three-neck flask equipped with a water separator, reflux condenser, thermometer and magnet, add 200ml of benzene, and react at 100°C for 12 hours. After the reaction, cool down to room temperature, and slowly add 0.06mol of CS to the reaction flask dropwise. 2 , then reacted at 80°C for 12 hours, evaporated the solvent under reduced pressure, washed the viscous liquid at the bottom several times with n-hexane, recrystallized with benzene, filtered with suction, and dried to obtain 50.3 g of light yellow crystals, with a yield of 71.2%.

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Abstract

Relating to a preparation method of spiro-compounds, the invention provides a phosphorus-containing spiro-compound and a preparation method thereof. The preparation method comprises the steps of: 1. reacting phosphorus-containing diol with di-n-butyltin oxide under certain conditions to generate an intermediate; 2. reacting the intermediate with carbon disulfide under certain conditions, carrying out pump filtration, washing, recrystallization and drying treatment, thus obtaining a phosphorus-containing spiro-compound product. The phosphorus-containing spiro-compound prepared in the invention can be used in epoxy resin, phenolic resin and other high polymer materials to improve the mechanical properties of polymer materials, and also can enhance the flame retardant property of the materials, thus being a multifunctional modification additive. The method adopted in the invention has the advantages of simple production process conditions, high product purity and yield, and easy aftertreatment process, etc.

Description

technical field [0001] The invention relates to a chemically synthesized spiro compound and a preparation method thereof, in particular to a phosphorus-containing spiro compound and a preparation method thereof. Background technique [0002] Since polymer materials were applied in industrial production in the late 1930s, they have been widely used in aviation, industry, national defense, medicine and other industries due to their excellent performance. But there is a common problem in the developed polymer materials: the performance of its practical application is far from its theoretical performance. This situation is caused by the stress concentration caused by the uneven force inside the material. There are many factors affecting stress concentration, the most important of which is the internal stress caused by volume shrinkage during polymerization. The existence of this destructive factor makes the adhesive joint inside the polymer matrix or between the resin matrix a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574
Inventor 王长松洪臻宁志高曹俊梁兵
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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