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Flame retardant phenylsilicic acid bisthiophosphatrioxacyclooctyl-4-methyl ester compound and preparation method thereof

A technology of phenylsilicic acid and trioxabicyclo, which is applied in the field of flame retardant phenylsilicic acid bisthiophosphatrioxacyclooctyl-4-methyl ester compound and its preparation, can solve the problem of life-threatening Property safety, fire and other issues, to achieve the effects of stable physical and chemical properties, good compatibility, and high decomposition temperature

Active Publication Date: 2018-06-19
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of these polymer materials are flammable and often cause fires, which seriously threaten the safety of people's lives and property.

Method used

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  • Flame retardant phenylsilicic acid bisthiophosphatrioxacyclooctyl-4-methyl ester compound and preparation method thereof
  • Flame retardant phenylsilicic acid bisthiophosphatrioxacyclooctyl-4-methyl ester compound and preparation method thereof
  • Flame retardant phenylsilicic acid bisthiophosphatrioxacyclooctyl-4-methyl ester compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1 In a 250mL four-necked reaction flask equipped with a stirrer, a thermometer and a hydrogen chloride absorption device, nitrogen was used to drive out the air, and at a temperature of 25°C, 27.46g (0.14mol) of 1-thiophospha-4- Hydroxymethyl-2,6,7-trioxabicyclo[2.2.2]octane and 140ml ethylene glycol dimethyl ether, slowly add 10.58g (0.05mol) phenyltrichlorosilane dropwise, and control the system with the dropping speed The temperature is not higher than 30°C. After the drop is completed, keep it at 50°C for 9 hours; then add distilled water that is equimolar to phenyltrichlorosilane dropwise, raise the temperature to 100°C, and keep it for 2 hours. After the HCl gas is released, add dropwise Adjust the pH of the system to 5-6 with 1.0 g of triethylamine, remove the organic solvent by distillation under reduced pressure, then add 120 mL of ethanol to make slurry for 1 hour, filter with suction, and dry to obtain white solid powder bis-1-thiophospha-2 phenylsilic...

Embodiment 2

[0027] Example 2 In a 250mL four-necked reaction flask equipped with a stirrer, a thermometer and a hydrogen chloride absorption device, nitrogen was used to drive out the air, and at a temperature of 25°C, 22.54g (0.115mol) of 1-thiophospha-4- Hydroxymethyl-2,6,7-trioxabicyclo[2.2.2]octane and 120ml dioxane, slowly add 10.58g (0.05mol) phenyltrichlorosilane dropwise, control system temperature with dropping rate If the temperature is higher than 30°C, keep it at 80°C for 8 hours after dropping; then add distilled water which is equimolar to phenyltrichlorosilane, raise the temperature to 100°C, and keep it for 2 hours. After the HCl gas is released, add 1.5g dropwise Adjust the pH of the system to 5-6 with dimethylaniline, remove the organic solvent by distillation under reduced pressure, then add 80 mL of methanol for beating for 1 hour, filter with suction, and dry to obtain bis-1-thiophospha-2 phenylsilicate as a white solid powder. The yield of 6,7-trioxabicyclo[2.2.2]oct...

Embodiment 3

[0028]Example 3 In a 250mL four-necked reaction flask equipped with a stirrer, a thermometer and a hydrogen chloride absorption device, nitrogen was used to drive out the air, and at a temperature of 25°C, 39.23g (0.20mol) of 1-thiophospha-4- Hydroxymethyl-2,6,7-trioxabicyclo[2.2.2]octane and 180ml ethylene glycol dimethyl ether, slowly add 10.58g (0.05mol) phenyltrichlorosilane dropwise, and control the system by dropping speed The temperature is not higher than 30°C. After the drop is completed, keep it at 40°C for 10 hours; then add distilled water that is equimolar to phenyltrichlorosilane dropwise, raise the temperature to 100°C, and keep it for 2 hours. After the HCl gas is released, add dropwise Adjust the pH of the system to 5-6 with 1.0 g of pyridine, remove the organic solvent by distillation under reduced pressure, then add 140 mL of ethanol to make slurry for 1 hour, filter with suction, and dry to obtain white solid powder of bis-1-thiophospha-2,6 phenylsilicate ,...

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Abstract

The invention relates to a flame retardant benzene siliconic acid bis-1-thiophospha-2,6,7-trioxabicyclo[2.2.2]octyl-4-methyl ester compound and a preparation method thereof. The compound is structurally shown as a formula in the description. The preparation method includes dissolving 1-thiophospha-4-hydroxymethyl-2,6,7- trioxabicyclo[2.2.2]octane into an organic solvent, and dropwise adding phenyl trichlorosilane to react for 6-10 hours at 40-100 DEG C; adding distilled water, and reacting for 2 hours at 100 DEG C; purifying so as to obtain the benzene siliconic acid bis-1-thiophospha-2,6,7-trioxabicyclo[2.2.2]octyl-4-methyl ester. The flame retardant has the advantages of high flame retarding efficiency and good char forming effect, thereby being suitably used as a flame-retardant charring agent for polyester, polyurethane, epoxy resin and unsaturated polyester resin. The preparation method has the advantages of simple production technology, low cost and easiness for industrialized production.

Description

technical field [0001] The present invention relates to a kind of synergistic flame retardant of three elements of silicon, phosphorus and sulfur, phenylsilicate dithiophosphatrioxa cage cyclooctyl-4-methyl ester compound and its preparation method, in particular to phenylsilicate bis -1-thiophospha-2,6,7-trioxabicyclo[2.2.2]octyl-4-methyl ester compound and its preparation method, the compound is suitable for polyester, polyurethane, epoxy resin, Flame retardant char forming agent for unsaturated resin etc. Background technique [0002] With the development of science and technology, synthetic polymer materials have been widely used in various fields. Most of these polymer materials are flammable and often cause fires, which seriously threaten people's lives and properties. In order to solve the flammability of synthetic materials and ensure the safety of synthetic materials, the most effective way is to add flame retardants. The use of halogen-based flame retardants is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6574C08K5/5419C08L67/00C08L75/04C08L63/00C08L67/06
CPCC07F9/65748C08K5/5419C08L2201/02C08L67/00C08L75/04C08L63/00C08L67/06
Inventor 沈东杰杨海军王令端孙艳艳
Owner SUZHOU UNIV OF SCI & TECH
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