Flame retardant bis[tris(2,3-dichloropropoxy)silicon-acyloxy]ethane compound and preparation method thereof

A technology of dichloropropoxy and silyloxy, which is applied in the direction of silicon organic compounds, can solve problems such as difficulty in finding, and achieve the effects of low production cost, low volatility, and good plasticity

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

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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  • Flame retardant bis[tris(2,3-dichloropropoxy)silicon-acyloxy]ethane compound and preparation method thereof
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  • Flame retardant bis[tris(2,3-dichloropropoxy)silicon-acyloxy]ethane compound and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0032]Embodiment 1 In the 250ml four-necked flask that stirrer, thermometer and high-efficiency reflux condenser are housed, and drying tube is housed on the condenser upper mouth, 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 to reduce the temperature of the reaction system to below 25°C, add 12.9g (9.47ml, 0.1mol) of 2,3-dichloropropanol dropwise , the dropwise addition process controls the reaction temperature not to be higher than 35°C. After the drop is completed, the temperature is raised to 45°C, and the temperature is kept for 2 hours; after the HCl gas is released, 3.1g (2.78ml, 0.05mol) of ethylene glycol is dropped into the In the flask, the reaction temperature was controlled by the dropping rate to not be higher than 55°C. After the drop, the temperature was raised to 65°C, and the reaction was carried out for 10 hours; , 0.201mol) 2,3-dic...

Embodiment 2

[0033] Example 2 In a 250ml four-necked 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 acetonitrile and 17g (11.47ml , 0.1mol) silicon tetrachloride, under stirring, cooled with a cold water bath, the temperature of the reaction system was reduced to below 25°C, 12.9g (9.47ml, 0.1mol) 2,3-dichloropropanol was added dropwise, and The process controls the reaction temperature not to be higher than 35°C. After dripping, raise the temperature to 45°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 55°C with the dropping speed, raise the temperature to 70°C after dropping, react for 9h, after the HCl gas is released, cool the system down to below 50°C, add dropwise 27.09g (19.90ml, 0.21mol ) 2,3-dichloropropanol, the ...

Embodiment 3

[0034] Example 3 In a 250ml four-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, and a drying tube at the top of the condenser, replace the air in the bottle with nitrogen, and add 60ml of ethylene glycol dimethyl ether and 17g (11.47ml, 0.1mol) of silicon tetrachloride, under stirring, cooled with a cold water bath to lower the temperature of the reaction system below 25°C, and dropwise added 12.9g (9.47ml, 0.1mol) of 2,3-dichloro Propanol, the dropwise addition process controls the reaction temperature not to be higher than 35°C. After the drop is completed, raise the temperature to 45°C and keep it warm for 2 hours; after the HCl gas is released, add 3.1g (2.78ml, 0.05mol) ethylene glycol dropwise In a four-necked flask, the reaction temperature is controlled at a rate of addition not higher than 55°C. After the drop is completed, the temperature is raised to 80°C, and the reaction is carried out for 7 hours. After the HCl gas is rel...

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Abstract

The invention relates to a flame retardant bis[tris(2,3-dichloropropoxy)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 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 glycol of a mole which is 0.5 times that of silicon tetrachloride, heating to the temperature of 65-80 DEG C after completing dripping, and reacting for 7-10 hours; 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 6-9 hours at the temperature of 70-90 DEG C; then, adding an acid binding agent, and carrying out heat preservation for 1 hour while stirring; purifying, thereby obtaining the flame retardant bis[tris(2,3-dichloropropoxy)silicon-acyloxy]ethane. The compound disclosed by the invention has high flame retarding efficacy due to the synergism of silicon and chlorine 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(2,3-dichloropropoxy)silyloxy]ethane compound and a preparation method thereof. The compound silicon and chlorine double elements have synergistically good flame retardant performance , 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 halogenated flame retardants burn , has be...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/04C08K5/5415C08L27/06
Inventor 王彦林董信
Owner SHANDONG XINGQIANG CHEM IND TECH RES INST CO LTD
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