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Fire retardant alkyl silicic acid trithio phosphonia trioxa bicyclo[2.2.2]octyl methyl ester compound and preparation method thereof

A technology of trioxabicyclo and flame retardant alkane, which is applied in the field of flame retardant alkyl silicate trithiophosphatrioxabicyclo[2.2.2]octyl methyl ester compound and its preparation, and can solve the problem of processing Poor performance and other problems, to achieve the effect of excellent flame retardant effect, simple equipment, and simple preparation process

Inactive Publication Date: 2017-03-15
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Phosphorus and halogen synergistic flame retardant research and application is early, but the use of phosphorus-halogen system is limited because of the halogen; phosphorus and nitrogen synergistic system has good flame retardant effect, but most of them have poor processability and other shortcomings

Method used

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  • Fire retardant alkyl silicic acid trithio phosphonia trioxa bicyclo[2.2.2]octyl methyl ester compound and preparation method thereof
  • Fire retardant alkyl silicic acid trithio phosphonia trioxa bicyclo[2.2.2]octyl methyl ester compound and preparation method thereof
  • Fire retardant alkyl silicic acid trithio phosphonia trioxa bicyclo[2.2.2]octyl methyl ester compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Example 1 In a 250mL four-necked reaction flask equipped with a stirrer, a thermometer and a fractionation device, nitrogen was used to drive out the air, and 6.81g (0.05mol) of methyltrimethoxysilane and 35.31g (0.18mol) of 1-thiol were added Phospha-4-hydroxymethyl-2,6,7-trioxabicyclo[2.2.2]octane, first heat up to 100°C, fractionation reaction for 5h; then heat up to 140°C, fractionation reaction for 10h, during the reaction Keep a slight vacuum (-0.02Mpa) in the bottle so that the generated methanol can be separated in time; after the reaction is completed, cool down to about 40°C, add 110mL of methanol and stir for 1h, then filter with suction and dry to obtain white solid powder formazan Tris-1-thiophospha-2,6,7-trioxabicyclo[2.2.2]octyl-4-methyl silicic acid ester with a yield of 93.1%.

Embodiment 2

[0036] Example 2 In a 250mL four-necked reaction flask equipped with a stirrer, a thermometer and a fractionation device, nitrogen was used to drive out the air, and 6.81g (0.05mol) of methyltrimethoxysilane and 39.23g (0.2mol) of 1-thiol Phospha-4-hydroxymethyl-2,6,7-trioxabicyclo[2.2.2]octane, first heated to 100°C, fractionated for 4 hours; then heated to 140°C, fractionated for 8 hours, during the reaction Keep a slight vacuum (-0.02Mpa) in the bottle so that the generated methanol can be separated in time; after the reaction is completed, cool down to about 40°C, then add 130mL of ethanol to stir and disperse for 1 hour, filter with suction, and dry to obtain white solid powder formazan Tris-1-thiophospha-2,6,7-trioxabicyclo[2.2.2]octyl-4-methyl silicic acid ester with a yield of 93.0%.

Embodiment 3

[0037] Example 3 In a 250mL four-necked reaction flask equipped with a stirrer, a thermometer and a fractionation device, nitrogen was used to drive out the air, and 6.81g (0.05mol) of methyltrimethoxysilane and 32.37g (0.165mol) of 1-thiol Phospha-4-hydroxymethyl-2,6,7-trioxabicyclo[2.2.2]octane, first heated to 100°C, fractionated for 3 hours; then heated to 160°C, fractionated for 6 hours, during the reaction Keep a slight vacuum (-0.02Mpa) in the bottle so that the generated methanol can be separated in time; after the reaction is completed, cool down to about 40°C, then add 80mL of ethanol to stir and disperse for 1 hour, filter with suction, and dry to obtain white solid powder formazan Tris-1-thiophospha-2,6,7-trioxabicyclo[2.2.2]octyl-4-methyl silicic acid ester with a yield of 92.7%.

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Abstract

The invention relates to a fire retardant alkyl silicic acid trithio phosphonia trioxa bicyclo[2.2.2]octyl methyl ester compound and a preparation method thereof. A structural formula of the compound is as shown in the specification, wherein R refers to CH3, CH3CH2 or CH3CH2CH2. The preparation method includes: performing reaction of alkyl trimethoxy silane or alkyltrichlorosilane with 1-thiophosphonia-4-hydroxymethyl-2,6,7-trioxa bicyclo[2.2.2]octane, and purifying to obtain alkyl silicic acid tri-1-thiophosphonia-2,6,7-trioxa bicyclo[2.2.2]octyl-4-methyl ester. The fire retardant is high in fire retardation efficiency, great in charring effect and suitable for serving as a fire-retardant charring agent for polyesters, polyurethanes, epoxy resin, unsaturated polyester resin and the like, and technical simplicity in production, low cost and easiness for industrial production are realized.

Description

technical field [0001] The invention relates to a synergistic flame retardant of silicon, phosphorus and sulfur three elements, alkyl silicate tri-1-thiophospha-2,6,7-trioxabicyclo[2.2.2]octyl-4-methanol An ester compound and a preparation method thereof, the compound is suitable for use as a flame-retardant char-forming agent for polyester, polyurethane, epoxy resin, unsaturated resin and the like. Background technique [0002] In practical applications, flame retardants containing only a single flame retardant element have more or less various deficiencies, and it is difficult to meet the flame retardant requirements of different materials, so compounding technology has been developed. At the same time, the research on intramolecular multi-element synergistic high-efficiency flame retardants has also become a trend in the development of flame retardant technology. Phosphorus and halogen synergistic flame retardant research and application is earlier, but the use of phosph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574C08K5/548C08K5/3492C08L67/00C08L75/04C08L63/00C08L101/00C08L67/02
CPCC07F9/65748C08K5/34928C08K5/548C08L2201/02C08L67/02
Inventor 沈东杰杨海军王令端孙艳艳
Owner SUZHOU UNIV OF SCI & TECH
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