Flame retardant bis[tri(3-chloropropoxy)silyloxy]ethane compound and preparation method thereof

A chloropropoxy and silicyloxy technology, applied in the direction of silicon organic compounds, can solve problems such as fire, threats to people's life and property safety, etc., and achieve low production cost, good application and development prospects, and good compatibility. Effect

Active Publication Date: 2015-11-25
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

[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 bis[tri(3-chloropropoxy)silyloxy]ethane compound and preparation method thereof
  • Flame retardant bis[tri(3-chloropropoxy)silyloxy]ethane compound and preparation method thereof
  • Flame retardant bis[tri(3-chloropropoxy)silyloxy]ethane compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 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 condenser, replace the air in the bottle with nitrogen, add 60ml of dichloroethane and 17g (11.47ml, 0.1mol) of silicon tetrachloride, under stirring, cooled with a cold water bath, so that the temperature of the reaction system was lowered to below 20°C, 9.454g (8.36ml, 0.1mol) of 3-chloropropanol was added dropwise, and The process controls the reaction temperature not to be higher than 30°C. After dropping, raise the temperature to 40°C and keep it warm for 2 hours; after the HCl gas is released, drop 3.1g (2.78ml, 0.05mol) of ethylene glycol into the four-necked flask , control the reaction temperature not higher than 50°C with the dropping speed, raise the temperature to 60°C after dropping, and react for 8h; ) 3-chloropropanol, the reaction temperature is controlled by the dropping rate not higher than 55°C, after the drop, t...

Embodiment 2

[0031]Example 2 In a 250ml 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 60ml carbon tetrachloride and 17g (11.47ml, 0.1mol) of silicon tetrachloride, under stirring, cooled with a cold water bath, so that the temperature of the reaction system was lowered to below 20°C, 9.454g (8.36ml, 0.1mol) of 3-chloropropanol was added dropwise, and The process controls the reaction temperature not to be higher than 30°C. After dropping, raise the temperature to 40°C and keep it warm for 2 hours; after the HCl gas is released, drop 3.1g (2.78ml, 0.05mol) of ethylene glycol into the four-necked flask , control the reaction temperature not higher than 50°C with the rate of addition, raise the temperature to 55°C after the drop, and react for 9 hours; after the HCl gas is released, cool the system down to below 40°C, add dropwise 19.85g (17.56ml, 0.21mol ) 3-c...

Embodiment 3

[0032] Example 3 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 60ml of dioxane and 17g (11.47ml, 0.1mol) of silicon tetrachloride, under stirring, cooled with a cold water bath, so that the temperature of the reaction system was lowered to below 20°C, 9.454g (8.36ml, 0.1mol) of 3-chloropropanol was added dropwise, and The process controls the reaction temperature not to be higher than 30°C. After dropping, raise the temperature to 40°C and keep it warm for 2 hours; after the HCl gas is released, drop 3.1g (2.78ml, 0.05mol) of ethylene glycol into the four-necked flask , control the reaction temperature not higher than 50°C with the dropping speed, raise the temperature to 70°C after the drop, and react for 6h; after the HCl gas is released, cool the system down to below 40°C, add dropwise 20.80g (18.39ml, 0.22mol ) ...

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Abstract

The invention relates to a flame retardant bis[tris(3-chloropropoxy)silicon-acyloxy]ethane 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 glycol of a mole which is 0.5 times that of silicon tetrachloride, heating to the temperature of 55-75 DEG C after completing dripping, and reacting for 5-9 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 6-9 hours at the temperature of 65-85 DEG C; adding an acid binding agent after HCl gas is completely discharged, and carrying out heat preservation for 1 hour while stirring; purifying, thereby obtaining the flame retardant bis[tris(3-chloropropoxy)silicon-acyloxy]ethane. The compound disclosed by the invention has high flame retarding efficacy due to the synergism of silicon and chlorine elements 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 bis[tri(3-chloropropoxy)silyloxy]ethane compound and a preparation method thereof. The compound can be used as polyvinyl chloride, unsaturated polyester, polyurethane and epoxy Flame retardant for materials such as resins. 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, that is, towards high effi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/04C08L27/06C08K5/5415
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
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