Triazinetri-tri(chloropropyl) silicate compound and preparation method thereof

A technology of triazine trisilicate tri-ester compound, which is applied in the field of flame retardant plasticizer, can solve the problems of long non-halogenation of flame retardants, and the process of non-halogenation will not be too fast, and achieve stable molecular structure and good environment. Benefit, good compatibility

Active Publication Date: 2012-10-17
张家港市乐余科创园投资发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the general development trend is: although the call for non-halogenation is high, the process of non-haloge

Method used

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  • Triazinetri-tri(chloropropyl) silicate compound and preparation method thereof
  • Triazinetri-tri(chloropropyl) silicate compound and preparation method thereof
  • Triazinetri-tri(chloropropyl) silicate compound and preparation method thereof

Examples

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Example Embodiment

[0029] Example 1 In a 100mL three-necked flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, 10ml of acetonitrile and 3.40ml of SiCl were added 4 (0.03mol). Dissolve 3.00g (0.01mol) triglycidyl isocyanurate in 50ml acetonitrile, drop it into a three-necked flask at 25°C, and control the dripping process to control the reaction temperature to not higher than 30°C. The addition is complete After that, the temperature was raised to 60°C for 1 hour and the reaction was kept for 4 hours; the reaction system was reduced to 30°C, and 11.61g (0.09mol) 2-chloropropanol was added dropwise. The temperature of the system was raised to 60℃ and the reaction was kept for 6h. Add about 0.5g of triethylamine, adjust to PH=5-6, stir for 1h, filter, the filtrate will distill the organic solvent (recycled), and then distill a small amount of low-boiling substances under reduced pressure , Get three {2-chloro-3-[tris(2-chloropropoxy)silanyloxy]propyl}isocyanurate, t...

Example Embodiment

[0030] Example 2 In a 100mL three-necked flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, 10ml of dichloroethane and 3.40ml of SiCl were added 4 (0.03mol), dissolve 3.00g (0.01mol) triglycidyl isocyanurate in 50ml dichloroethane, drop it into a three-necked flask at 25℃, and control the reaction temperature during the dropping process. When the temperature is higher than 30℃, after the addition is completed, the temperature is raised to 60℃ for 1h and the reaction is kept for 6h; the reaction system is reduced to 30℃, and 12.26g (0.095mol) 2-chloropropanol is added dropwise, and the reaction temperature is controlled to not exceed 4 at the rate of dripping. After the dripping is finished, the temperature of the system is increased to 60℃ for 6h, and about 0.5g N,N-dimethylaniline is added, adjusted to PH=5-6, stirred for 1h, filtered, and the filtrate is evaporated to remove the organic solvent and Excess 2-chloropropanol (recycled for use), a...

Example Embodiment

[0031] Example 3 In a 100mL three-necked flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, 10ml of tetrahydrofuran and 3.40ml of SiCl were added 4 (0.03mol). Dissolve 3.00g (0.01mol) triglycidyl isocyanurate in 50ml tetrahydrofuran, drop it into a three-necked flask at 25℃, control the dripping process, the reaction temperature is not higher than 30℃, and the addition is complete After that, the temperature was raised to 60°C for 1 hour and the temperature was kept for 5 hours; the reaction system was reduced to 30°C, and 12.9g (0.10mol) 2-chloropropanol was added dropwise. The reaction temperature was controlled at the rate of dropping to not exceed 40°C. After the addition, The temperature of the system was raised to 50℃ and the reaction was kept for 5h. Add about 0.5g of melamine, adjust to PH=5-6, stir for 1h, filter, the filtrate will distill the organic solvent and excess 2-chloropropanol (recycled), and then reduce pressure Distill a sm...

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Abstract

The invention relates to a silicon-halogen synergic flame retardant triazinetri-tri(chloropropyl) silicate compound and a preparation method thereof, in particular to a tri{2-chloro-3-[tri(chloropropoxy)siacryloxy]propyl}isocyanurate compound and a preparation method thereof. The compound has the structural formula shown in the specification, wherein OC3H6Cl is OCH2CHClCH3 or OCH2CH2CH2Cl or OCH(CH3)CH2Cl. The preparation method comprises the following steps of: controlling a certain molar ratio of raw materials; enabling triepoxypropylisocyanurate to react with silicon tetrachloride at 60 DEG C for 4-6 hours in an organic solvent; adding epoxypropane and reacting at 50-60 DEG C for 4-6 hours; and purifying to obtain the product triazinetri-tri(chloropropyl) silicate. The triazinetri-tri(chloropropyl) silicate provided by the invention has good flame-retardant plasticizing property and is suitable to be used as a flame-retardant plasticizer of polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin and the like; and the production technology is simple, the cost is low, and the industrial production is easy to realize.

Description

technical field [0001] The invention relates to a triazine trisilicate tris(chloropropyl) ester compound and a preparation method thereof, in particular to a tris{2-chloro-3-[tris(chloropropoxy)silyloxy]propyl }isocyanurate compound and its preparation method. The compound is a three-element synergistic flame-retardant plasticizer of nitrogen, silicon, and chlorine, and is suitable for flame-retardant plasticizers of polyvinyl chloride, polyurethane, epoxy resin, and unsaturated resin. plasticizer. Background technique [0002] With the world's increasingly stringent flame retardant legislation, the successive introduction of industry directives and the increasing awareness of environmental protection, the global consumption of flame retardants is showing a rapid growth trend, especially the more urgent demand for new, efficient and environmentally friendly flame retardants. [0003] At present, halogen-based flame retardants are the two types of organic flame retardants wit...

Claims

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Application Information

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IPC IPC(8): C07F7/04C08K5/544C08L27/06
Inventor 王彦林王红霞吴娟
Owner 张家港市乐余科创园投资发展有限公司
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