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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-halogenation will not be too fast, that is, the non-halogenation of flame retardants will be a relatively long process

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

Experimental program
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Effect test

Embodiment 1

[0029] Example 1 In a 100mL three-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, add 10ml of acetonitrile, 3.40ml of SiCl 4 (0.03 mol). Dissolve 3.00g (0.01mol) triglycidyl isocyanurate in 50ml of acetonitrile, drop it into a three-necked flask at 25°C, control the reaction temperature not higher than 30°C during the dropping process, and complete the dropwise addition After that, heat up to 60°C for 1h and keep it warm for 4h; lower the reaction system to 30°C, add 11.61g (0.09mol) 2-chloropropanol dropwise, and control the reaction temperature to not exceed 40°C at the rate of addition. Raise the temperature of the system to 60°C and keep it warm for 6 hours, add about 0.5g of triethylamine, adjust to PH = 5-6, stir for 1 hour, filter, distill off the organic solvent from the filtrate (for recycling), and distill out a small amount of low boiling point substances under reduced pressure , to get three {2-chloro-3-[three (2-chloropro...

Embodiment 2

[0030] Example 2 In a 100mL three-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, add 10ml of dichloroethane, 3.40ml of SiCl 4(0.03mol), 3.00g (0.01mol) of triglycidyl isocyanurate was dissolved in 50ml of dichloroethane, and at 25°C, it was dropped into the three-necked bottle, and the dropping process controlled the reaction temperature to If the temperature is higher than 30°C, after the dropwise addition is completed, heat up to 60°C for 1h and keep the temperature for 6h; lower the reaction system to 30°C, add 12.26g (0.095mol) 2-chloropropanol dropwise, and control the reaction temperature by the rate of addition to not exceed 4 ℃, after the dropwise addition, raise the temperature of the system to 60℃ and keep it warm for 6h, add about 0.5g N,N-dimethylaniline, adjust to PH=5-6, stir for 1h, filter, and distill the filtrate to remove the organic solvent and Excess 2-chloropropanol (recycled for use), and then evaporate a small a...

Embodiment 3

[0031] Example 3 In a 100mL three-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, add 10ml tetrahydrofuran, 3.40ml SiCl 4 (0.03 mol). Dissolve 3.00g (0.01mol) triglycidyl isocyanurate in 50ml tetrahydrofuran, drop it into a three-necked flask at 25°C, control the reaction temperature not higher than 30°C during the dropping process, and complete the dropwise addition After that, heat up to 60°C for 1h and keep the temperature for 5h; lower the reaction system to 30°C, add 12.9g (0.10mol) of 2-chloropropanol dropwise, and control the reaction temperature at a rate of addition not to exceed 40°C. After the dropwise addition, the Raise the temperature of the system to 50°C and keep it warm for 5 hours, add about 0.5g of melamine, adjust to PH=5-6, stir for 1 hour, filter, distill off the organic solvent and excess 2-chloropropanol (recycled) from the filtrate, and then depressurize A small amount of low-boilers were evaporated to obtain ...

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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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