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Preparation method of flame retardant cyke tris(dimethyl-1,3-dihalopropoxysilicate) ester compound

A technology of dihalopropoxysilicic acid and dimethyldichlorosilane, applied in the field of flame retardant plasticizers, can solve problems such as limitations, and achieve the effects of large molecular weight, good compatibility and good stability

Active Publication Date: 2018-04-20
HUZHOU RUIGAO NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, its application in some fields is limited because of the harmful gas released during high-temperature combustion; silicon-based flame retardants have attracted much attention because of their excellent flame retardant properties, good processing properties, and especially environmental friendliness; nitrogen Flame retardants are the focus of the development of intumescent flame retardants

Method used

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  • Preparation method of flame retardant cyke tris(dimethyl-1,3-dihalopropoxysilicate) ester compound
  • Preparation method of flame retardant cyke tris(dimethyl-1,3-dihalopropoxysilicate) ester compound
  • Preparation method of flame retardant cyke tris(dimethyl-1,3-dihalopropoxysilicate) ester compound

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Effect test

Embodiment 1

[0036] Embodiment 1 In the 250ml four-necked bottle that stirrer, thermometer and condensation tube are equipped with, and drying tube and hydrogen chloride absorption device are equipped with at the top of condensation tube, replace the air in the bottle with nitrogen, add 8.74g (0.0333mol ) Trihydroxyethylisocyanurate and 100ml dioxane, add 12.91g (0.1mol) dimethyldichlorosilane, heat up to 70°C, keep warm for 5h; after the HCl gas is released, cool down to 30°C Below ℃, add 12.9g (0.1mol) 1,3-dichloro-2-propanol dropwise, control the reaction temperature not higher than 40℃ with the dropping speed, raise the temperature to 90℃ after dropping, keep the reaction for 8h; wait for HCl gas After the release, add 0.3g of 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 80ml of petroleum ether, stir for 0.5h, stand still, and separate the ...

Embodiment 2

[0037] Embodiment 2 In the 250ml four-necked bottle that stirrer, thermometer and condensation tube are equipped with, and drying tube and hydrogen chloride absorption device are equipped with on the top of condensation tube, replace the air in the bottle with nitrogen, add 8.74g (0.0333mol ) trihydroxyethyl isocyanurate and 140ml tetrahydrofuran, add 12.91g (0.1mol) dimethyldichlorosilane, heat up to 50°C, keep warm for 9 hours; after the HCl gas is released, cool down to below 30°C, Add 13.76g (0.1067mol) 1,3-dichloro-2-propanol dropwise, control the reaction temperature not higher than 40°C at the rate of addition, raise the temperature to 60°C after dropping, and keep it warm for 12 hours; after the HCl gas is released , add 0.5g melamine, adjust the pH of the system to 5~6, filter with suction, distill the filtrate under reduced pressure to remove solvent, excess 1,3-dichloro-2-propanol and a small amount of low boiling point substances, then add 100ml petroleum ether, sti...

Embodiment 3

[0038] Embodiment 3 In the 250ml four-necked bottle that stirrer, thermometer and condensation tube are housed, and drying tube and hydrogen chloride absorption device are equipped with at the top of condensation tube, replace the air in the bottle with nitrogen, add 8.74g (0.0333mol ) trihydroxyethyl isocyanurate and 100ml diethylene glycol dimethyl ether, add 12.91g (0.1mol) dimethyldichlorosilane, heat up to 55°C, and keep it warm for 8 hours; after the HCl gas is released, Cool down to below 30°C, add 15.05g (0.1167mol) of 1,3-dichloro-2-propanol dropwise, control the reaction temperature not higher than 40°C at the rate of addition, raise the temperature to 110°C after dropping, and keep warm for 6 hours; After the HCl gas is released, add 1 g of 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 1,3-dichloro-2-propanol and a small amount of low boiling point substances, and then ...

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Abstract

The present invention relates to a kind of preparation method of flame retardant Sike tris(dimethyl-1,3-dihalopropoxysilicate) ester compound, the structure of the compound is shown in the following formula: where Q=Cl or Br . The preparation method is: under the protection of nitrogen, react dimethyldichlorosilane or dimethyldibromosilane with trihydroxyethyl isocyanurate in an organic solvent at 40°C-70°C for 4-9h, Then add 1,3-dihalo-2-propanol dropwise, and react at 50°C-110°C for 6-12 hours; )ester. The flame retardant of the invention has high flame retardant efficiency and good char formation effect, is suitable for use as a flame retardant plasticizer for polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin, etc., and has simple production process, low cost and easy industrialization Production.

Description

technical field [0001] The invention relates to a method for preparing a synergistic flame retardant of silicon, nitrogen and halogen three-element sike tris(dimethyl-1,3-dihalopropoxysilicate) ester compound, which is suitable for use as polyvinyl chloride , polyurethane, epoxy resin, unsaturated resin and other flame retardant plasticizers. Background technique [0002] After the synthetic polymer materials are widely used, because most of them are flammable, they must be modified by flame retardancy to have satisfactory fire resistance and ensure the safety of use. Among them, halogenated flame retardants have been widely used due to their high flame retardant performance and excellent comprehensive cost performance. However, its application in some fields is limited because of the harmful gas released during high-temperature combustion; silicon-based flame retardants have attracted much attention because of their excellent flame retardant properties, good processing pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18C08K5/5465C08K5/544
Inventor 王彦林王州厅杨海军
Owner HUZHOU RUIGAO NEW MATERIALS CO LTD
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