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A kind of preparation method of silicon, nitrogen, halogen synergistic flame retardant plasticizer

A technology of synergistic flame retardant and plasticizer, which is applied in the preparation of flame retardant plasticizer triisocyanurate compound and the field of flame retardant plasticizer, which can solve the problem of narrow use range, limitation, and the price of silicon-based flame retardants. Advanced problems, to achieve the effect of low cost, large molecular weight, good application development prospects

Active Publication Date: 2018-08-21
HUZHOU RUIGAO NEW MATERIALS CO LTD
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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 char formation, but generally silicon-based flame retardants are limited by their high price and narrow use range.

Method used

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  • A kind of preparation method of silicon, nitrogen, halogen synergistic flame retardant plasticizer
  • A kind of preparation method of silicon, nitrogen, halogen synergistic flame retardant plasticizer
  • A kind of preparation method of silicon, nitrogen, halogen synergistic flame retardant plasticizer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035]Example 1 In a 250ml four-necked bottle equipped with a stirrer, a thermometer and a condenser tube, and a drying tube on the top of the condenser tube, replace the air in the bottle with nitrogen, and add 9.91g (0.0333mol) of isocyanurate Acetate triglycidyl ester, 70ml dioxane and 12.91g (0.1mol) dimethyldichlorosilane, heat up to 90°C for 1h, keep warm for 6h; cool down to below 40°C, connect a hydrogen chloride absorption device to the drying tube, Add 8.05g (0.1mol) 2-chloroethanol dropwise, control the reaction temperature not higher than 60°C with the dropping rate, raise the temperature to 100°C after dropping, and keep the temperature for 4 hours; after the HCl gas is released, add 0.25g melamine to adjust The pH of the system was 5-6, suction filtered, and the filtrate was distilled off under reduced pressure to remove the solvent and a small amount of low-boiling matter to obtain tris(dimethylchloroethoxysilyloxychloropropyl)isocyanurate with a yield of 93.3% ...

Embodiment 2

[0036] Example 2 In a 250ml four-necked bottle equipped with a stirrer, a thermometer and a condenser tube, and a drying tube on the top of the condenser tube, replace the air in the bottle with nitrogen, and add 9.91g (0.0333mol) of isocyanurate Acid triglycidyl ester, 50ml diethylene glycol dimethyl ether and 12.91g (0.1mol) dimethyl dichlorosilane, heat up to 100°C for 1h, keep the temperature for 5h; cool down to below 40°C, connect hydrogen chloride to the drying tube Absorption device, add 8.59g (0.1067mol) 2-chloroethanol dropwise, control the reaction temperature not higher than 60°C with the drop rate, raise the temperature to 70°C after dropping, keep the reaction for 8h; after the HCl gas is released, add 0.5g Melamine, adjust the pH of the system to 5-6, filter with suction, and distill the filtrate under reduced pressure to remove the solvent, excess 2-chloroethanol (recycled) and a small amount of low boiling point matter to obtain tris(dimethylchloroethoxysilylox...

Embodiment 3

[0037] Example 3 In a 250ml four-necked bottle equipped with a stirrer, a thermometer and a condenser tube, and a drying tube on the top of the condenser tube, replace the air in the bottle with nitrogen, and add 9.91g (0.0333mol) of isocyanurate Acetate triglycidyl ester, 100ml acetonitrile and 12.91g (0.1mol) dimethyl dichlorosilane, heat preservation reaction at 70°C for 8h; lower the temperature to below 40°C, connect a hydrogen chloride absorption device to the drying tube, add dropwise 9.39g ( 0.1167mol) of 2-chloroethanol, the reaction temperature is controlled by the dropping rate not higher than 60°C, after the dropping, the temperature is raised to 90°C, and the reaction is kept for 6 hours; after the HCl gas is released, add 0.8g of melamine to adjust the pH of the system to 5~ 6. Suction filtration, the filtrate is distilled off under reduced pressure to remove the solvent, excess 2-chloroethanol (recycled) and a small amount of low boiling point matter to obtain tr...

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Abstract

The invention relates to a preparation method of a plasticizer with collaborative flame retardancy of silicon, nitrogen and halogen and in particular relates to a preparation method of tris (dimethyl halogen ethoxy silicon acyloxy halogen propyl). The structure of the compound is shown in the specification. In the formula, when m=0, n=1; when m=1, n=0; Q=Cl or Br; and X=Cl or Br. The preparation method comprises the following steps: dissolving triglycidyl isocyanurate in an organic solvent, adding 3 times mole of dimethyldichlorosilane, raising the temperature to 40-100 DEG C, and carrying out heat preservation reaction for 5-10h; and adding 3-4 times mole of 2-halohydrins dropwise, reacting for 4-10h at the temperature of 60-100 DEG C, and purifying to obtain the tris (dimethyl halogen ethoxy silicon acyloxy halogen propyl). The flame retardant plasticizer is high in flame-retarded efficiency, good in compatibility with a polymer material, suitable for being used as the flame retardant plasticizer of polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin and the like, simple in production process, low in cost and easy in realizing industrial production.

Description

technical field [0001] The invention relates to a preparation method of a silicon, nitrogen and halogen synergistic flame retardant plasticizer, in particular to a flame retardant plasticizer tris(dimethylhaloethoxysilyloxyhalopropyl)isocyanuric acid The preparation method of the ester compound is suitable for use as a flame-retardant plasticizer of polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin and the like. Background technique [0002] The wide application of flammable polymer materials has promoted 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 flammable due to the addition of plasticizers. At present, there is a strong urgency in the market for new high-efficiency, low-toxicity, and low-cost flame-retardant plasticizers....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18C08K5/544C08K5/5455
Inventor 王彦林杨海军周瑞华
Owner HUZHOU RUIGAO NEW MATERIALS CO LTD
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