Method for preparing silicon, nitrogen and halogen multielement synergistic fire retardant compound

A synergistic flame-retardant, dimethyl dihalopropoxysilyloxyhalopropyl technology, which is applied in the field of isocyanurate triester preparation, can solve the problem of lower mechanical properties of substrates, moisture-absorbing processing properties, Low flame retardant efficiency and other issues, to achieve excellent flame retardant effect, strong water resistance, and good compatibility

Active Publication Date: 2015-07-01
HUZHOU RUIGAO NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main way of preliminary halogen-free flame retardant is to add magnesium hydroxide, aluminum hydroxide, zinc borate and expanded graphite to the base material, but because of its low flame retardant efficiency, a large amount of filling is required to achieve better flame retardant effect, tends to reduce the mechanical properties of the base material
In addition, although phosphorus-nitrogen flame retardants have high flame retardant efficiency, most of them have shortcomings such as easy migration, easy moisture absorption, and poor processing performance.
Therefore, although the call for halogen-free is increasing day by day, the development of halogen-free flame retardants at this stage is still difficult to meet the needs of society, and halogen-based flame retardants will still occupy an important position in the field of flame retardancy

Method used

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  • Method for preparing silicon, nitrogen and halogen multielement synergistic fire retardant compound
  • Method for preparing silicon, nitrogen and halogen multielement synergistic fire retardant compound
  • Method for preparing silicon, nitrogen and halogen multielement synergistic fire retardant compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030]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 21.79g (0.1mol) of 1,3-dibromo-2-propanol dropwise, and control the reaction temperature not higher than 60°C at the rate of addition, raise the temperature to 100°C after dropping, and keep the reaction for 6 hours; after the HCl gas is released , add 0.4g melamine, adjust the pH of the system to 5-6, filter with suction, distill the filtrate under reduced pressure to remove the solvent and a small amount of low boiling point substances, then add 30ml of petroleum ether, stir for 0.5h, let stand, separate the lower lay...

Embodiment 2

[0031] 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 Acetate triglycidyl ester, 100ml acetonitrile and 21.8g (0.1mol) dimethyldibromosilane, heat up to 80°C, keep warm for 7 hours; cool down to below 40°C, connect the hydrogen bromide absorption device to the drying tube, drop 23.25g (0.1067mol) 1,3-dibromo-2-propanol, control the reaction temperature not higher than 60°C at the rate of addition, raise the temperature to 80°C after the drop, keep the temperature for 7 hours; after the HBr gas is released, add 1g of melamine, adjust the pH of the system to 5-6, filter with suction, distill the filtrate under reduced pressure to remove the solvent, excess 1,3-dibromo-2-propanol (recycled) and a small amount of low boiling point matter, then add 50ml petroleum ether, Stir for 0.5h, let it ...

Embodiment 3

[0032] 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 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 25.43g (0.1167mol) 1,3-dibromo-2-propanol dropwise, control the reaction temperature not higher than 60°C at the rate of addition, raise the temperature to 110°C after dropping, keep warm for 5 hours; wait for HCl gas After the release, add 1.2g of melamine, adjust the pH of the system to 5-6, filter with suction, and distill off the filtrate under reduced pressure to remove the solvent, excess 1,3-dibromo-2-propanol (recycled for use) and a small amount of low boiling point matter, Th...

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Abstract

The invention relates to a method for preparing a silicon, nitrogen and halogen multielement synergistic fire retardant compound. The structure of the compound is shown in a formula which can be seen in the specification; in the formula, when m is 1, n is 0; when m is 0, n is 1; X is Cl or Br; Y is Cl or Br; OC3H5Y2 is OCH(CH2Br)2, OCH2CHBrCH2Br, OCH(CH2Cl)2 or OCH2CHClCH2Cl. The preparation method comprises the following steps: in an organic solvent, reacting triglycidyl isocyanurate with dimethyl dihalogenosilane for 5-8h at the temperature of 70-100 DEG C, dropwise adding dihalogen propyl alcohol, reacting for 5-8h at the temperature of 70-110 DEG C, and purifying to obtain t isocyanuric acid tri(dimethyl dihalogen propoxy silicane acyloxy propyl halide)ester. The fire retardant provided by the invention is high in fire retarding efficiency, good in char forming effect and is suitable for being used as a fire retardant plasticizer for polyvinyl chloride, polyurethane, epoxy resin and unsaturated resin; in addition, the production process is simple, the cost is low and the industrial production can be easily realized.

Description

technical field [0001] The invention relates to a preparation method of a silicon, nitrogen and halogen multi-element synergistic flame retardant compound, in particular to a preparation method of tris(dimethyldihalopropoxysilyloxyhalopropyl) isocyanurate. The compound is suitable as a flame retardant plasticizer for polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin, etc. Background technique [0002] With the promotion of the European Union's implementation of flame retardant and non-halogenated regulations on electronic products, my country introduced the corresponding flame retardant regulations on July 1, 2007, which greatly promoted the research and development of new varieties of flame retardants in my country. The main way of preliminary halogen-free flame retardant is to add magnesium hydroxide, aluminum hydroxide, zinc borate and expanded graphite to the base material, but because of its low flame retardant efficiency, a large amount of filling is req...

Claims

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Application Information

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IPC IPC(8): C07F7/18C08K5/544C08L27/06
Inventor 王彦林张元新杨海军
Owner HUZHOU RUIGAO NEW MATERIALS CO LTD
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