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Caged bicyclic phosphate siloxane flame retardant and preparation method thereof

A technology of phosphate ester siloxane and phosphate ester, which is applied in the field of flame retardants, can solve the problems of large amount of addition, poor heat resistance, and easy precipitation, etc., and achieve the effect of mild reaction conditions, high thermal stability, and easy availability of raw materials

Active Publication Date: 2011-08-17
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The phosphorus-containing organosilicon flame retardant synthesized by the above patents has the following disadvantages: low phosphorus content, poor heat resistance, insufficient flame retardant efficiency, high polarity, easily soluble in water or common organic solvents, and easy to precipitate
[0017] However, in these flame retardants containing PEPA groups, only one element, phosphorus, acts as a flame retardant, resulting in insufficient flame retardant efficiency and a large amount of addition

Method used

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  • Caged bicyclic phosphate siloxane flame retardant and preparation method thereof
  • Caged bicyclic phosphate siloxane flame retardant and preparation method thereof
  • Caged bicyclic phosphate siloxane flame retardant and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0035] The preparation of tris(2,6,7-trioxa-1-oxyphosphabicyclo[2.2.2]octane-4-methyleneoxy)silane (TRPSi): under the protection of nitrogen, the Add 180.0g (1.0mol) of PEPA, 79.1g (1.0mol) of pyridine and 200mL of acetonitrile into the reaction kettle with stirring, reflux condensing device, heating device and drying protection device, and raise the temperature to 30°C. After the PEPA is dissolved, use a constant pressure funnel to 44.4 g (0.33 mol) of trichlorosilane was added dropwise within 1 h. After the addition was completed, the reaction was carried out at 30° C. for 2 h, and then the temperature was raised to 82° C. for 5 h under reflux. Stop the reaction and cool to room temperature, filter, wash the filter residue with chloroform and water until there is no chloride ion, and obtain 156.9 g of the product after vacuum drying, with a yield of 84.0%.

[0036] product 1 HNMR (DMSO-d6), δ: 4.55~4.71 (18H, d, endomethylene), 3.76~3.89 (6H, d, exomethylene), 3.13~3.17 (1H...

Embodiment 2

[0038] Preparation of three (2,6,7-trioxa-1-oxyphosphabicyclo[2.2.2]octane-4-methyleneoxy)silane (TRPSi): under the protection of nitrogen gas, the Add 180.0g (1.0mol) of PEPA, 49.3g (0.30mol) of triethoxysilane, 500mL of dimethyl sulfoxide into the reaction kettle of mechanical stirring, distillation device, heating device and drying protection device, raise the temperature to 100°C, and The ethanol produced by the reaction was continuously collected. After 10 hours of reaction, the reaction was stopped and cooled to room temperature, and 200 mL of 1,4-dioxane was added and stirred to precipitate the product. The filter residue was washed with acetonitrile and water until there was no chloride ion, and 102.9 g of the product was obtained after vacuum drying with a yield of 60.6%.

[0039] product 1 H NMR (DMSO-d6), δ: 4.53~4.75 (18H, d, endomethylene), 3.75~3.93 (6H, d, exomethylene), 3.10~3.21 (1H, t, silicon atom ).

Embodiment 3

[0041] Preparation of methyltris (2,6,7-trioxa-1-oxyphosphabicyclo[2.2.2]octane-4-methyleneoxy)silane (MTPSi): under nitrogen protection, Add 180.0g (1.0mol) of PEPA, 79.1g (1.0mol) of pyridine, 1g of magnesium chloride and 500mL of chloroform into the reaction kettle with mechanical stirring, reflux condensing device, heating device and drying protection device. , Add 44.8g (0.3mol) methyltrichlorosilane dropwise within 1h with a constant pressure funnel, after the addition is complete, keep the reaction at 60°C for 1h, then raise the temperature to 62°C for reflux reaction for 8h. Stop the reaction and cool to room temperature, filter, wash the filter residue with chloroform and water until there is no chloride ion, and obtain 135.4 g of the product after vacuum drying, with a yield of 77.8%.

[0042] product 1H NMR (DMSO-d6), δ: 4.52~4.67 (18H, d, endomethylene), 3.79~3.94 (6H, d, exomethylene), 1.29~1.34 (3H, m, methyl ).

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Abstract

The invention discloses a caged bicyclic phosphate siloxane flame retardant and a preparation method thereof. A structural formula of the caged bicyclic phosphate siloxane flame retardant is shown in a general formula (I). During the preparation, the needed product can be obtained by reacting 1-oxophospha-4-hydroxymethyl-2,6,7-trioxabicyclo[2.2.2]octane and chlorosilane or alkoxy silane. A plurality of rigid caged bicyclic phosphate groups and silicon element which are contained in the compound play a role in synergistic flame retardancy; and the flame retardant has higher thermal stability and carbon-forming performance, and can effectively reduce the smoke produced in the combustion.

Description

technical field [0001] The invention relates to a novel flame retardant, in particular to a siloxane flame retardant containing multiple bicyclic cage phosphate groups and a preparation method thereof, belonging to the field of flame retardants. Background technique [0002] Silicone flame retardants are a new type of halogen-free flame retardants, which have the advantages of non-toxicity, low smoke, and anti-dripping. However, the flame retardant effect of using silicone flame retardants alone is mostly not ideal. Utilizing the synergistic flame retardant effect between phosphorus and silicon, introducing phosphorus into organosilicon molecules is one of the ways to obtain new high-efficiency flame retardants. In recent years, researchers have synthesized a variety of phosphorus-containing silicone flame retardants, including: [0003] U.S. Patent US 4093641 synthesized a phosphorus-containing methoxysilane with a structural formula of: [0004] [0005] Chinese paten...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574C09K21/06
Inventor 赵建青陈俊刘述梅
Owner SOUTH CHINA UNIV OF TECH
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