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Triazine chlorotrisilicate compound and preparation method thereof

A technology of trisilicate and triazine chloride, applied in the direction of silicon organic compounds, etc., can solve the problems of high price, narrow scope of use, restrictions, etc., and achieve the effects of low cost, good environmental benefits, and good symmetry characteristics

Active Publication Date: 2014-10-15
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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  • Triazine chlorotrisilicate compound and preparation method thereof
  • Triazine chlorotrisilicate compound and preparation method thereof
  • Triazine chlorotrisilicate compound and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0028] 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, the temperature will rise to 60°C within 1 hour, keep the temperature for 4 hours, then lower the temperature of the system to 40°C, add 8.33g dropwise (0.09mol) 2,3-dichloropropanol, after dripping, heat up to 50°C, keep warm for 6 hours, add about 0.5g triethanolamine dropwise, adjust to PH=5-6, stir for 1 hour, filter, and distill out the filtrate Organic solvent (recycling), then distill off excess 2,3-dichloropropanol (recycling) and a small amount of low boiling point under reduced pressure to obtain a colorless or light yellow liquid tri{2-chloro-3-[three ( 2,3-Dic...

Embodiment 2

[0029]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) dichloroethane solution of triglycidyl isocyanurate 50ml, control the temperature of the system to not 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 temperature of the system to 40°C ℃, add 9.25 (0.10mol) 2,3-dichloropropanol dropwise, after dropping, raise the temperature to 60°C, keep warm for 6 hours, add about 0.5g N,N-dimethylaniline dropwise, adjust to PH=5 -6, stirred for 1h, filtered, the filtrate was distilled to remove the organic solvent (for recycling), and then distilled off excess 2,3-dichloropropanol (for recycling) and a small amount of low boiling point matter under reduced pressure to ob...

Embodiment 3

[0030] 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, 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 40°C ℃, add 10.18g (0.11mol) dichloropropanol dropwise, after dropping, raise the temperature to 70°C, keep warm for 5h, add about 0.5g pyridine dropwise, adjust to PH=5-6, stir for 1h, filter, and distill the filtrate Remove the organic solvent (for recycling), then distill off excess 2,3-dichloropropanol (for recycling) and a small amount of low boiling point substances under reduced pressure to obtain a colorless or pale yellow liq...

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Abstract

The invention relates to a tris(2-chloro-3-[tris (dichloropropoxy) silicon acyloxy] propyl) isocyanurate fire retardant compound and a preparation method of the compound. The compound has a structure shown in the specification. The preparation method comprises the following steps: adding isocyanurate triglycidyl to silicon tetrachloride according to a certain mole ratio and carrying out thermal-insulation reacting for 4-5h at 60 DEG C; then dropwise adding dichloropropanol according to a certain mole ratio and carrying out thermal-insulation reaction for 4-6h at 50-70 DEG C; and finally purifying to obtain the tris(2-chloro-3-[tris(dichloropropoxy) silicon acyloxy] propyl) isocyanurate. The compound is an excellent fire retardant plasticizer and the production process is simple, low in equipment investiment and is suitable for industrial production.

Description

technical field [0001] The invention relates to a triazine chlorotrisilicate compound and a preparation method thereof, in particular to a tri{2-chloro-3-[tri(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] Due to the wide application of flammable polymer materials, the research of flame retardant technology and the rapid development of flame retardant plasticizer industry have been promoted. 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 flammable due to the addition of plasticizers. At present, there is a strong urgency in the market for new high-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/04C08K5/544C08K13/02C08L27/06
Inventor 王彦林杨海李豫丹
Owner 张家港市乐余科创园投资发展有限公司
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