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Flame retardant bis[tris(1,3-dichloro-2-propoxy)silyloxy]ethane compound and preparation method thereof

A technology of silyloxy and flame retardant, applied in the direction of silicon organic compounds, etc., can solve problems such as difficulty in finding, and achieve the effects of low production cost, good plasticity, and high synergistic flame retardant efficiency

Active Publication Date: 2016-04-27
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

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Problems solved by technology

Since the European Union announced in 1986 that polybrominated diphenyl ether flame retardants produced carcinogen dioxin when burned, the use of halogenated flame retardants has been restricted. It has become an important research direction of halogenated flame retardants to research and develop high-efficiency halogenated flame retardants to reduce the amount of flame retardants and reduce their toxicity.

Method used

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  • Flame retardant bis[tris(1,3-dichloro-2-propoxy)silyloxy]ethane compound and preparation method thereof
  • Flame retardant bis[tris(1,3-dichloro-2-propoxy)silyloxy]ethane compound and preparation method thereof
  • Flame retardant bis[tris(1,3-dichloro-2-propoxy)silyloxy]ethane compound and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Embodiment 1 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 60ml acetonitrile and 17g (11.47ml , 0.1mol) silicon tetrachloride, under stirring, cool with cold water bath, make reaction system temperature drop below 25 ℃, dropwise add 12.9g (9.55ml, 0.1mol) 1,3-dichloro-2-propanol , 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 open flask, control the reaction temperature not higher than 55°C with the rate of addition, and raise the temperature to 65°C after dropping, and react for 10 hours; , 0.201mol) 1,3-dichloro-2-propanol, the reaction temperature is c...

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 to lower the temperature of the reaction system below 25°C, and dropwise added 12.9g (9.55ml, 0.1mol) of 1,3-dichloro-2 -Propanol, the reaction temperature is controlled not to be higher than 35°C during the dropping process, after the drop is completed, the temperature is raised to 45°C, and the reaction is kept for 2 hours; after the HCl gas is released, 3.1g (2.78ml, 0.05mol) ethylene glycol is dropped Put it into a four-necked flask, control the reaction temperature not higher than 55°C at the rate of addition, raise the temperature to 70°C after the drop, and react for 9 hours; after the HCl gas is released, cool the system down to below 50°C, and ...

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 to lower the temperature of the reaction system below 25°C, and dropwise added 12.9g (9.55ml, 0.1mol) of 1,3-dichloro-2 -Propanol, the reaction temperature is controlled not to be higher than 35°C during the dropping process, after the drop is completed, the temperature is raised to 45°C, and the reaction is kept for 2 hours; after the HCl gas is released, 3.1g (2.78ml, 0.05mol) ethylene glycol is dropped Put it into a four-necked flask, control the reaction temperature not higher than 55°C with the dropping speed, raise the temperature to 80°C after dropping, and react for 7h; (21.01ml, 0.22mol) 1,3-dichloro-2-propanol, control the reaction ...

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Abstract

The invention relates to a flame retardant bis[tris(1,3-dichloro-2-propoxy)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 1,3-dichloro-2-propanol 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 1,3-dichloro-2-propanol of a mole which is 2-3 times that of silicon tetrachloride, and carrying out heat-preservation reaction for 6-10 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(1,3-dichloro-2-propoxy)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 facilitated.

Description

technical field [0001] The invention relates to a flame retardant bis[tri(1,3-dichloro-2-propoxy)silyloxy]ethane compound and a preparation method thereof. The compound is suitable for polyvinyl chloride, polyurethane, cyclo Flame retardant for materials such as oxygen resin and unsaturated resin. Background technique [0002] With the rapid development of the world economy, the continuous improvement of people's living standards and the enhancement of safety and fire prevention awareness, the flame retardant industry has developed rapidly, especially the research on new high-efficiency flame retardants is more urgent. Since the European Union announced in 1986 that polybrominated diphenyl ether flame retardants produced carcinogen dioxin when burned, the use of halogenated flame retardants has been restricted. The research and development of high-efficiency halogenated flame retardants to reduce the dosage of flame retardants and reduce their toxicity has become an importa...

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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