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Tri[2-tri(1,3-dichloroisopropoxy)silicon acyl oxyethyl]isocyanurate compound and preparation method thereof

A technology of trishydroxyethylisocyanurate and dichloroisopropoxy, which is applied in the direction of silicon organic compounds, can solve problems such as difficulty in finding substitutes, achieve high molecular weight, improve the difficulty of dispersion and low activity, and produce low cost effect

Active Publication Date: 2014-01-29
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

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. Therefore, research and development of high-efficiency halogenated flame retardants to reduce the amount of flame retardants and reduce their toxicity has become an important research direction for halogenated flame retardants

Method used

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  • Tri[2-tri(1,3-dichloroisopropoxy)silicon acyl oxyethyl]isocyanurate compound and preparation method thereof
  • Tri[2-tri(1,3-dichloroisopropoxy)silicon acyl oxyethyl]isocyanurate compound and preparation method thereof
  • Tri[2-tri(1,3-dichloroisopropoxy)silicon acyl oxyethyl]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 condensing tube, and a drying tube on the condensing tube upper mouth, replace the air in the bottle with nitrogen, add 20ml tetrachloroethane 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 25°C, and dropwise added 6.45g (4.78ml, 0.05mol) of 1,3-dichloro- 2-propanol, the dropwise addition process controls the reaction temperature not to be higher than 35°C. After the dropwise addition, raise the temperature to 45°C and keep the temperature for 2 hours; The ethyl chloride solution was dropped into a four-necked flask, and the reaction temperature was controlled by the dropping rate to not be higher than 65°C. After the drop, the temperature was raised to 90°C, and the reaction was carried out for 11 hours. After the HCl gas was released, the system was cooled to 50...

Embodiment 2

[0032] Example 2 In a 250ml four-necked flask equipped with a stirrer, a thermometer and a high-efficiency reflux condensing tube, and a drying tube on the condensing 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 25°C, and dropwise added 6.45g (4.78ml, 0.05mol) of 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 heat preservation reaction is carried out for 2 hours; Drop the solution of oxyhexane into the four-necked flask, control the reaction temperature not higher than 65°C with the dropping speed, raise the temperature to 90°C after the drop, react for 10 hours, and cool the system down to 50°C after the HCl gas is released Next, add 14.19g (10.51ml, 0.11...

Embodiment 3

[0033] Embodiment 3 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 20ml acetonitrile and 8.5g (5.67 ml, 0.05mol) 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 6.45g (4.78ml, 0.05mol) of 1,3-dichloro-2-propane Alcohol, 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 heat preservation reaction is carried out for 2 hours; Put it into a four-necked flask, control the reaction temperature at a rate of addition not higher than 65°C, raise the temperature to 80°C after the drop, and react for 13 hours. (11.46ml, 0.12mol) 1,3-dichloro-2-propanol, control the reaction temperature not higher than 65°C ...

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Abstract

The invention relates to a fire retardant, namely a tri[2-tri(1,3-dichloroisopropoxy)silicon acyl oxyethyl]isocyanurate compound, and a preparation method thereof; the structure of the compound is represented by a formula shown in the specification; the preparation method comprises the following steps: reacting silicon tetrachloride and equimolar 1,3-dichloro-2-propyl alcohol in an organic solvent below 25 DEG C, dropwise adding the organic solution of trihydroxyethyl isocyanurate the mol weight of which is 1 / 3 times of that of silicon tetrachloride, reacting at 80-95 DEG C for 9-13 hours, dropwise adding 1,3-dichloro-2-propyl alcohol the mol weight of which is 2-3 times of that of silicon tetrachloride, and reacting at 80-95 DEG C for 7-10 hours; adding an acid-binding agent, stirring and performing heat preservation for 1 hour; purifying to obtain the fire retardant, namely a tri[2-tri(1,3-dichloroisopropoxy)silicon acyl oxyethyl]isocyanurate compound. The compound disclosed by the invention has the advantages of being high in flame-retardant performance, simple in preparation process, low in cost and easy for industrial production and is applied to being used as the fire retardant of materials, such as polyvinyl chloride, polyurethane, epoxy resin and unsaturated resin.

Description

technical field [0001] The invention relates to a flame retardant tris[2-tris(1,3-dichloroisopropoxy)silyloxyethyl]isocyanurate compound and a preparation method thereof, the compound silicon, nitrogen and chlorine The three-element synergistic flame retardant has high performance and is suitable for use as a flame retardant for materials such as polyvinyl chloride, polyurethane, epoxy 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 demand for 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...

Claims

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Application Information

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IPC IPC(8): C07F7/04C08K5/5455C08K13/02C08L27/06
Inventor 王彦林董信
Owner SHANDONG XINGQIANG CHEM IND TECH RES INST CO LTD
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