Isocyanurate chloropropyl chloroethyl silicate and preparation method thereof

A technology of isocyanurate and isocyanuric acid tri, which is applied in the field of flame-retardant plasticizers, can solve the problems of limited use, narrow use range, and high price, and achieve good plasticization, low cost, and environmental protection. Effect

Active Publication Date: 2012-10-17
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, silicone-based products are generally expensive and have a narrow range of use, so their use is restricted.

Method used

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  • Isocyanurate chloropropyl chloroethyl silicate and preparation method thereof
  • Isocyanurate chloropropyl chloroethyl silicate and preparation method thereof
  • Isocyanurate chloropropyl chloroethyl silicate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1 In a 100ml three-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, add 10ml of acetonitrile, use nitrogen to exhaust the air in the bottle, and accurately draw 3.40ml (0.03mol) of SiCl 4 Placed in a three-neck bottle. Weigh 3.00g (0.01mol) of triglycidyl isocyanurate and dissolve it in 40ml of acetonitrile. Add the solution dropwise into a three-necked flask at 20°C for about 0.5h. Then lower the temperature to 30°C, install an extremely flexible and expandable soft sealing sleeve on the upper mouth of the high-efficiency reflux condenser, and inject 3.96g (0.09mol) of ethylene oxide under the liquid surface, and the temperature of the feeding process should not be higher than 40°C. Then heat up to 55°C for 3 hours of heat preservation reaction, and check that the pH of the reaction solution is at 5-6 as the end point. After the reaction is over, the solvent and low boiling point substances are distilled off under reduce...

Embodiment 2

[0026] Example 2 In a 100ml three-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, add 10ml of tetrahydrofuran, use nitrogen to drive out the air in the bottle, and accurately draw 3.40ml (0.03mol) of SiCl 4 Placed in a three-neck bottle. Weigh 3.00g (0.01mol) of triglycidyl isocyanurate and dissolve it in 40ml of tetrahydrofuran. Add the solution dropwise into a three-necked flask at 20°C for about 0.5h. Then lower the temperature to 30°C, install an extremely flexible and expandable soft sealing sleeve on the upper mouth of the high-efficiency reflux condenser, and inject 4.40g (0.10mol) of ethylene oxide under the liquid surface, and the temperature of the feeding process should not be higher than 40°C. Then heat up to 50°C for 3 hours of heat preservation reaction, and check that the pH of the reaction solution is at 5-6 as the end point. After the reaction is over, the solvent and low boiling point substances are distilled off unde...

Embodiment 3

[0027] Example 3 In a 100ml three-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, add 10ml of dioxane, use nitrogen to drive out the air in the bottle, and accurately draw 3.40ml (0.03mol) of SiCl 4Placed in a three-neck bottle. Weigh 3.00g (0.01mol) of triglycidyl isocyanurate and dissolve it in 40ml of dioxane, add the solution dropwise into a three-necked flask at 20°C for about 0.5h, and raise the temperature to 60°C for reaction 5h, then lower the temperature to 30°C, install an extremely flexible and inflatable soft sealing sleeve on the upper mouth of the high-efficiency reflux condenser, and inject 4.84g (0.11mol) of ethylene oxide under the liquid surface, and the temperature of the injection process should not be higher than 40 ℃, then heat up to 45 ℃ for 2 hours, and check that the pH of the reaction solution is at 5-6. Oxygen)silyloxy]propyl}isocyanurate, yield rate: 96.3%, flash point (open cup): 214±5°C, decomposition te...

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Abstract

The invention relates to a nitrogen, silicon and chlorine thee-element synergic flame retardant tri{2-chloro-3-[tri(chloroethoxy)silicon acyloxy]propyl}isocyanurate compound and a preparation method thereof. The structure of the compound is shown as a formula in the specification. The preparation method comprises the following steps: dripping organic solvent solution of triglycidyl Isocyanurate into silicon tetrachloride, and reacting for 4 to 6 hours at a temperature of between 50 and 70 DEG C; and cooling to 30 DEG C, introducing ethylene oxide under the liquid surface, reacting for 2 to 3 hours at a temperature of between 45 and 55 DEG C, and purifying to obtain the tri{2-chlor-3-[tri(chloroethoxy)silicon acyloxy]propyl}isocyanurate. The compound has good flame retardant plasticization, and is suitable for flame retardant plasticizer such as polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin and the like; and the method has simple production process and low cost, and is easy for industrial production.

Description

technical field [0001] The present invention relates to a synergistic flame retardant of three elements of nitrogen, silicon and chlorine and a preparation method thereof, in particular to a tri{2-chloro-3-[tri(chloro An ethoxy)silyloxy]propyl}isocyanurate compound and a preparation method thereof, the compound is suitable for use as a flame retardant plasticizer for polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin and the like. Background technique [0002] With the development of the national economy and the improvement of people's living standards, synthetic fibers, plastics, rubber and other polymer materials are more and more widely used in transportation, building materials, electronic appliances, daily furniture, interior decoration and other fields. However, these polymer materials are generally flammable and easy to cause fire accidents. In order to solve the problems of flame resistance and smoke suppression of synthetic materials and ensure the saf...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/04C08K5/5455C08L27/06
Inventor 王彦林楼晓莉李豫丹吴娟
Owner SUZHOU UNIV OF SCI & TECH
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