Flame retardant tris[2-tris(3-chloropropoxy)silicon-acyloxy-ethyl]isocyanurate compound and preparation method thereof

A technology of trihydroxyethyl isocyanurate and silicyloxyethyl is applied in the field of flame retardant tris[2-trisilyloxyethyl]isocyanurate compound and its preparation, and can Solve problems such as fire, threats to people's lives and property, and achieve the effects of low production cost, good application and development prospects, and low volatility

Active Publication Date: 2014-02-05
SHANDONG XINGQIANG CHEM IND TECH RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Because most of the widely used polymer materials are flammable, they often cause fires and pose a serious threat to people's lives and property.

Method used

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  • Flame retardant tris[2-tris(3-chloropropoxy)silicon-acyloxy-ethyl]isocyanurate compound and preparation method thereof
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  • Flame retardant tris[2-tris(3-chloropropoxy)silicon-acyloxy-ethyl]isocyanurate compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031]Example 1 In a 250ml four-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, and a drying tube on the upper mouth of the condenser, replace the air in the bottle with nitrogen, add 20ml of dichloroethane and 8.5 g (5.67ml, 0.05mol) of silicon tetrachloride, under stirring, cooled with a cold water bath to lower the temperature of the reaction system below 20°C, add 4.727g (4.18ml, 0.05mol) of 3-chloropropanol dropwise, During the addition process, the reaction temperature should not be higher than 30°C. After dripping, raise the temperature to 40°C, and keep it warm for 2 hours; Put it into a four-necked flask, control the reaction temperature not higher than 65°C at the rate of addition, raise the temperature to 80°C after the drop, and react for 11 hours; after the HCl gas is released, cool the system down to below 50°C, and add 9.55g (8.44ml, 0.101mol) 3-chloropropanol, control the reaction temperature not higher than 65°C with t...

Embodiment 2

[0032] Example 2 In a 25ml four-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, and a drying tube on the condenser, replace the air in the bottle with nitrogen, add 20ml carbon tetrachloride and 8.50 g (5.67ml, 0.05mol) of silicon tetrachloride, under stirring, cooled with a cold water bath to lower the temperature of the reaction system below 20°C, add 4.727g (4.18ml, 0.05mol) of 3-chloropropanol dropwise, During the addition process, the reaction temperature should not be higher than 30°C. After the dripping, raise the temperature to 40°C, and keep it warm for 2 hours; Put it into a four-necked flask, control the reaction temperature at a rate not higher than 65°C, raise the temperature to 75°C after the drop, and react for 12 hours. After the HCl gas is released, cool the system down to below 50°C, and add 10.4g (9.20ml, 0.11mol) 3-chloropropanol, control the reaction temperature not higher than 65°C with the rate of addition, after...

Embodiment 3

[0033] Example 3 In a 250ml four-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condensation tube, and a drying tube on the top of the condensation tube, replace the air in the bottle with nitrogen, and add 20ml of dioxane and 8.5 g (5.67ml, 0.05mol) of silicon tetrachloride, under stirring, cooled with a cold water bath to lower the temperature of the reaction system below 2o°C, add 4.727g (4.18m, 0.05mol) of 3-chloropropanol dropwise, During the addition process, the reaction temperature should not be higher than 30°C. After dripping, raise the temperature to 40°C, and keep it warm for 2 hours; Put it into a four-necked flask, control the reaction temperature not higher than 65°C at the rate of addition, raise the temperature to 90°C after the drop, and react for 8 hours; after the HCl gas is released, cool the system down to below 50°C, and add 11.34g (10.03ml, 0.12mol) 3-chloropropanol, control the reaction temperature not higher than 65°C a...

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Abstract

The invention relates to a flame retardant tris[2-tris(3-chloropropoxy)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 3-chloropropanol of a mole which is equal to that of silicon tetrachloride in an organic solvent at the temperature below 20 DEG C, then, dropwise adding an organic solution of trishydroxyethyl isocyanurate of a mole which is 1 / 3 that of silicon tetrachloride, heating to the temperature of 75-90 DEG C after completing dripping, reacting for 8-12 hours, then, dropwise adding 3-chloropropanol 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 75-90 DEG C; then, adding an acid binding agent, and carrying out heat preservation for 1 hour while stirring; purifying, thereby obtaining the flame retardant tris[2-tris(3-chloropropoxy)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(3-chloropropoxy)silyloxyethyl]isocyanurate compound and a preparation method thereof. The compound can be used as polyvinyl chloride, unsaturated polyvinyl chloride Flame retardant for materials such as esters, polyurethanes and epoxies. Background technique [0002] Because most of the widely used polymer materials are flammable, they often cause fires and pose a serious threat to people's lives and properties. With the rapid development of science and technology in our country and the continuous improvement of people's living standards, people's safety awareness has gradually increased, thus promoting the development of flame-retardant materials and flame-retardant technologies. Due to the environmental hazards of halogenated flame retardants during combustion, they have been questioned by the society. In recent years, stricter requirements have been put forward for halogenated flame retardants,...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): C07F7/04C08K5/5455C08L27/06C08L67/06C08L75/04C08L63/00
Inventor王彦林董信
OwnerSHANDONG XINGQIANG CHEM IND TECH RES INST CO LTD