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

A technology of chloropropoxy and silyloxy, applied in the direction of silicon organic compounds, etc., can solve the problems of high cost performance of halogen-based flame retardants, difficult to find substitutes, release of harmful gases, etc., and achieve good application and development. Prospects, overcoming the effect of volatile reaction and low volatility

Active Publication Date: 2015-12-02
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

Traditional halogenated flame retardants have been developed earlier and their application technologies are relatively mature, but they release harmful gases during the combustion of materials, so they are limited in some application fields
Due to the high overall cost performance of halogenated flame retardants, it is still difficult to find completely suitable substitutes

Method used

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

Examples

Experimental program
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Effect test

Embodiment 1

[0034]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 60ml of dioxane and 17g (11.47ml, 0.1mol) of silicon tetrachloride, under stirring, cooled with a cold water bath, the temperature of the reaction system was reduced to below 20°C, and 9.454g (8.48ml, 0.1mol) of chloropropanol was added dropwise, and the dropping process was controlled The reaction temperature is not higher than 30°C. After dripping, raise the temperature to 40°C and keep the temperature for 2 hours; The dropping rate controls the reaction temperature not to be higher than 50°C. After the dropping, the temperature is raised to 75°C and reacted for 6 hours; after the HCl gas is released, the temperature of the system is lowered to below 40°C, and 20.80g (18.65ml, 0.22mol) of chlorine is added dropwise For propanol, the reaction temperature...

Embodiment 2

[0035] 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 upper mouth of 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, the temperature of the reaction system was reduced to below 20°C, and 9.454g (8.48ml, 0.1mol) of chloropropanol was added dropwise, and the dropping process was controlled The reaction temperature is not higher than 30°C. After dripping, raise the temperature to 40°C and keep the temperature for 2 hours; The dropping speed controls the reaction temperature not to be higher than 50°C. After the dropping, the temperature is raised to 60°C and reacted for 8 hours; after the HCl gas is released, the temperature of the system is lowered to below 40°C, and 19g (17.04ml, 0.201mol) of chloropropane is added dropwise Alcohol, control the react...

Embodiment 3

[0036] 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 acetonitrile and 17g (11.47ml , 0.1mol) of silicon tetrachloride, under stirring, cooled with a cold water bath, the temperature of the reaction system was reduced to below 20°C, and 9.454g (8.48ml, 0.1mol) of chloropropanol was added dropwise, and the reaction temperature was controlled during the dropwise addition process. If the temperature is 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, controlled by the dropping rate The reaction temperature is not higher than 50°C. After the dripping, the temperature is raised to 65°C and reacted for 7 hours; after the HCl gas is released, the temperature...

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Abstract

The invention relates to a fire retardant 2[3(chlorine propoxy)silicon acyloxy] ethane compound and a preparation method thereof. The structure of the compound is shown in the specification; -OC3H6Cl in the formula is 2-chlorin-1-propoxy or 1-chlorin-2-propoxy or a mixture of the 2-chlorin-1-propoxy and the 1-chlorin-2-propoxy. The preparation method comprises the following steps: dropwise adding equimolar chloropropanol to an organic solvent of silicon tetrachloride below 20 DEG C to react for 2 hours at 40 DEG C; then dropwise adding ethylene glycol which is 0.5fold mole of the silicon tetrachloride to react for 6-9 hours at 55-75 DEG C; cooling to below 40 DEG C; dropwise adding chloropropanol which is 2-3fold mole of the silicon tetrachloride to react for 6-10 hours at 65-85 DEG C; adding a little of acid-binding agent, and stirring for 1 hour in heat preservation, thereby obtaining fire retardant 2[3(chlorine propoxy)silicon acyloxy] ethane by purification treatment. The compound disclosed by the invention is applicable to being used as a fire retardant of the materials such as polyvinyl chloride, polyurethane, epoxy resin and unsaturated polyester resin, and is simple in preparation technology and low in cost, and easily achieves industrial production.

Description

technical field [0001] The invention relates to a flame retardant bis[tri(chloropropoxy)silyloxy]ethane compound and a preparation method thereof. The compound can be used as polyvinyl chloride, unsaturated polyester, polyurethane and epoxy resin, etc. Flame retardant for materials. Background technique [0002] Due to the extensive use of flammable organic synthetic polymer materials, the research and development of flame retardant materials and technologies have been promoted. Traditional halogenated flame retardants have been developed earlier and their application technologies are relatively mature, but they release harmful gases during the combustion of materials, so they are limited in some application fields. Due to the high overall cost performance of halogenated flame retardants, it is still difficult to find completely suitable substitutes. Research and develop multi-element synergistic high-efficiency halogen flame retardants, reduce the amount of flame retardan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/04C08K5/5415C08L27/06C08L67/06C08L75/04C08L63/00
Inventor 王彦林董信
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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