Tris[2-tris(2,3-dichloropropoxy)silyloxyethyl]isocyanurate compound and preparation method thereof

A technology of silyloxyethyl and dichloropropoxy, applied in the direction of silicon organic compounds, can solve problems such as difficulty in finding, and achieve the effects of large molecular weight, good plasticity and good compatibility

Active Publication Date: 2016-04-06
山东产研中科高端化工产业技术研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current development status of flame retardants is that with the increasingly stringent flame retardant legislation around the world, the introduction of fire safety standards, the successive introduction of industry directives, and the increasing calls for environmental protection, due to the toxic gas generated when halogenated flame retardants burn , has been restricted in many aspects, but due to the excellent comprehensive cost performance of halogenated flame retardants, it is still difficult to find suitable substitutes in many aspects. Research and development of high-efficiency halogenated flame retardants has become one of the important research directions

Method used

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  • Tris[2-tris(2,3-dichloropropoxy)silyloxyethyl]isocyanurate compound and preparation method thereof
  • Tris[2-tris(2,3-dichloropropoxy)silyloxyethyl]isocyanurate compound and preparation method thereof
  • Tris[2-tris(2,3-dichloropropoxy)silyloxyethyl]isocyanurate compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032]Example 1 In a 250ml four-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condensing tube, and a drying tube at the top of the condensing tube, replace the air in the bottle with nitrogen, add 20ml of dioxane and 8.5 g (5.67ml, 0.05mol) of silicon tetrachloride, under stirring, cooled with a cold water bath to reduce the temperature of the reaction system to below 25°C, add 6.45g (4.74ml, 0.05mol) of 2,3-dichloropropane dropwise Alcohol, the dropwise addition process controls the reaction temperature not to be higher than 35°C. After the dropwise addition, raise the temperature to 45°C and keep it warm for 2 hours; drop the solution into a four-necked flask, and control the reaction temperature at a rate not higher than 65°C. After the drop, the temperature was raised to 90°C and reacted for 10 hours. Add 14.19g (10.42ml, 0.11mol) of 2,3-dichloropropanol, and control the reaction temperature not to be higher than 65°C at the rate of additio...

Embodiment 2

[0033] Example 2 In a 250ml four-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condensing tube, and a drying tube on the top of the condensing tube, replace the air in the bottle with nitrogen, add 20ml tetrachloroethane and 8.5 g (5.67ml, 0.05mol) of silicon tetrachloride, under stirring, cooled with a cold water bath to reduce the temperature of the reaction system to below 25°C, add 6.45g (4.74ml, 0.05mol) of 2,3-dichloropropane dropwise Alcohol, the dropwise addition process controls the reaction temperature not to be higher than 35°C. After the dropwise addition, raise the temperature to 45°C and keep it warm for 2 hours; Drop the solution into a four-necked flask, and control the reaction temperature at a rate not higher than 65°C. After the drop, the temperature is raised to 90°C and reacted for 11 hours. After the HCl gas is released, the system is cooled to below 50°C. Add 13.029g (9.57ml, 0.101mol) of 2,3-dichloropropanol, and control...

Embodiment 3

[0034] Embodiment 3 In the 250ml four-necked flask that stirrer, thermometer and high-efficiency reflux condenser are equipped with, and drying tube is housed on the condenser upper mouth, replace the air in the bottle with nitrogen, add 20ml acetonitrile and 8.5g (5.67 ml, 0.05mol) of silicon tetrachloride, under stirring, cooled with a cold water bath to lower the temperature of the reaction system below 25°C, add 6.45g (4.74ml, 0.05mol) of 2,3-dichloropropanol dropwise, dropwise During the addition process, the reaction temperature should not be higher than 35°C. After dripping, raise the temperature to 45°C, and keep it warm for 2 hours; In the open flask, the reaction temperature is controlled by the dropping rate to not be higher than 65°C. After the drop is completed, the temperature is raised to 80°C, and the reaction is carried out for 13 hours. , 0.12mol) 2,3-dichloropropanol, the reaction temperature is controlled by the rate of addition not to be higher than 65°C, ...

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Abstract

The invention relates to a flame retardant tris[2-tris(2,3-dichloropropoxy)silicon-acyloxy-ethyl]isocyanurate compound and a preparation method thereof. The structure of the compound is represented by a formula shown in a drawing. The preparation method comprises the steps of reacting silicon tetrachloride with 2,3-dichloropropanol of a mole which is equal to that of silicon tetrachloride in an organic solvent at the temperature below 25 DEG C, then, dropwise adding an organic solution of trishydroxyethyl isocyanurate of a mole which is 1 / 3 that of silicon tetrachloride, reacting for 9-13 hours at the temperature of 80-95 DEG C, then, dropwise adding 2,3-dichloropropanol of a mole which is 2-3 times that of silicon tetrachloride, and carrying out heat-preservation reaction for 7-10 hours at the temperature of 80-95 DEG C; then, adding an acid binding agent, and carrying out heat preservation for 1 hour while stirring; purifying, thereby obtaining a product, namely the tris[2-tris(2,3-dichloropropoxy)silicon-acyloxy-ethyl]isocyanurate. The compound disclosed by the invention has high flame retarding efficacy and is suitable for serving as a flame retardant for materials, such as polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin and the like, and the preparation method is simple and is low in cost, so that the industrial production is easy to realize.

Description

technical field [0001] The invention relates to a flame retardant tris[2-tris(2,3-dichloropropoxy)silyloxyethyl]isocyanurate compound and a preparation method thereof, the compound silicon, nitrogen and chlorine The synergistic flame retardant performance of the elements is high, and it is suitable for use as a flame retardant for materials such as polyvinyl chloride, polyurethane, epoxy resin, and unsaturated resin. Background technique [0002] In recent years, the global market demand for flame retardants has been showing a rapid growth trend, especially the demand for new, efficient and environmentally friendly flame retardants is more urgent. The current development status of flame retardants is that with the increasingly stringent flame retardant legislation around the world, the introduction of fire safety standards, the successive introduction of industry directives, and the increasing calls for environmental protection, due to the toxic gas generated when halogenate...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C07F7/04C08K5/5455C08L27/06
Inventor王彦林杨海军董信
Owner山东产研中科高端化工产业技术研究院有限公司