Nitrogen-containing chloro-polysilicate compound and preparation method thereof

A silicate and compound technology, which is applied in the field of nitrogen-containing chloropolysilicate compound and its preparation, can solve the problems of limitation, high price, and narrow application range, and achieve low cost, high flame retardant efficiency, and good environment benefit effect

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

Silicon-based flame retardant plasticizers have attracted people's attention due to their excellent properties of suppressing smoke and promoting carbon formation. However, general silicon-based flame retardants are limited by their high price and narrow application range.

Method used

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  • Nitrogen-containing chloro-polysilicate compound and preparation method thereof
  • Nitrogen-containing chloro-polysilicate compound and preparation method thereof
  • Nitrogen-containing chloro-polysilicate compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1 Add 10ml of acetonitrile and 3.40ml (0.03mol) of silicon tetrachloride to a 100ml four-necked reaction flask equipped with a stirrer, a thermometer, and a high-efficiency reflux condenser, and add 3.00g (0.01mol) of isochloride dropwise at 25°C. 50ml of acetonitrile solution of triglycidyl cyanurate, the temperature of the system should not exceed 30°C at the rate of addition, after the drop is completed, the temperature will rise to 60°C within 1 hour, keep the temperature for 4 hours, then lower the temperature of the system to 50°C, and add 8.33g dropwise (0.09mol) epichlorohydrin, after dripping, be warming up to 70 ℃, insulation reaction 8h, when PH=5-6, reaction finishes, decompression distillation removes solvent (reuse) and a small amount of low boiling point matter, obtains Color liquid tris{2-chloro-3-[tris(dichloropropoxy)silyloxy]propyl}isocyanurate, the product yield is 96%. Its flash point (open cup): 240±5°C, decomposition temperature: 280±5°C, ...

Embodiment 2

[0026] Example 2 Add 10ml of dichloroethane, 3.40ml (0.03mol) of silicon tetrachloride in a 100ml four-necked reaction flask equipped with a stirrer, a thermometer, and a high-efficiency reflux condenser, and add 3.00g (0.01mol) of silicon tetrachloride dropwise at 25°C. mol) 50ml of dichloroethane solution of triglycidyl isocyanurate, control the system temperature not to exceed 30°C at the rate of addition, after the drop is completed, heat up to 60°C within 1 hour, keep the temperature for 5 hours, and then lower the system temperature to 50°C ℃, add 9.25 (0.10mol) epichlorohydrin dropwise, after dripping, heat up to 80 ℃, heat preservation reaction 8h, when PH=5-6, reaction finishes, solvent and excess epichlorohydrin ( reuse) and a small amount of low-boiling matter to obtain colorless liquid tris{2-chloro-3-[tri(dichloropropoxy)silyloxy]propyl}isocyanurate, and the product yield is 97% . Its flash point (open cup): 240±5°C, decomposition temperature: 280±5°C, density (2...

Embodiment 3

[0027] Example 3 Add 10ml of tetrachloroethane, 3.40ml (0.03mol) of silicon tetrachloride in a 100ml four-necked reaction flask equipped with a stirrer, a thermometer, and a high-efficiency reflux condenser, and add 3.00g (0.01mol) of silicon tetrachloride dropwise at 25°C. mol) 50ml of tetrachloroethane solution of triglycidyl isocyanurate, the temperature of the system is controlled to not exceed 30°C at the rate of addition, after the drop is completed, the temperature is raised to 60°C within 1 hour, and the temperature is kept for 5 hours, and then the temperature of the system is lowered to 50°C ℃, add 10.18g (0.11mol) epichlorohydrin dropwise, after dropping, raise the temperature to 90°C, keep the temperature for 7 hours, when PH=5-6, the reaction is over, and distill off the solvent and excess epichlorohydrin under reduced pressure (recycling) and a small amount of low boiling point matter, to obtain a colorless liquid three {2-chloro-3- [three (dichloropropoxy) silylo...

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Abstract

The invention relates to a tri{2-chloro-3-[tri(dichloropropoxy)silicon acyloxy]propyl}isocyanurate compound and a preparation method thereof. The structure of the compound is shown in the specification. The preparation method comprises the steps of adding triglycidyl isocyanurate in a certain molar ratio to silicon tetrachloride, preserving heat at 60 DEG C and reacting for 4-5 hours, then dropwise adding epoxy chloropropane in a certain molar ratio, preserving heat at 70-90 DEG C and reacting for 6-8 hours to obtain tri{2-chloro-3-[tri(dichloropropoxy)silicon acyloxy]propyl}isocyanurate through purification treatment. The compound is an excellent flame-retardant plasticizer; and the preparation method is simple in production process and low in equipment investment and is easy for industrial production.

Description

technical field [0001] The invention relates to a nitrogen-containing chloropolysilicate compound and a preparation method thereof, in particular to a tris{2-chloro-3-[tris(dichloropropoxy)silyloxy]propyl}isocyanate Urate compound and its preparation method. The compound is a three-element synergistic flame-retardant plasticizer of nitrogen, silicon, and chlorine, and is suitable for use as a flame-retardant plasticizer for polyvinyl chloride, polyurethane, epoxy resin, and unsaturated resin. Background technique [0002] With the wide application of polymer materials, because of its flammability, it often causes fires and poses a serious threat to people's lives and property, thus promoting the research of flame retardant technology and the rapid development of flame retardant plasticizer industry. Flame retardant plasticizer is a plastic processing aid with flame retardant function and plasticizing effect. It can overcome the problem of making polymer materials more flamm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/544C07F7/04C08L27/06C08L75/04C08L63/00C08L101/00
Inventor 王彦林李豫丹吴娟楼晓莉
Owner 张家港市乐余科创园投资发展有限公司
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