Flame retardant charring agent-tetra-{1-oxyphospha-2,6,7-trioxabicyclo-[2.2.2]-octane-(4)-methyl} silicate compound and preparation method thereof

A technology of ester compound and tetrasilicic acid, which is applied in the field of flame-retardant carbon-forming agent tetracage ring silicate PEPA ester compound and its preparation, can solve the problems of flammable materials, hidden dangers of life and property safety, etc., and achieve low cost and low cost. Good charcoal properties and novel structure

Active Publication Date: 2014-09-03
RES INST OF XIANGCHENG SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] With the development of polymer material science, plastics, rubber and fibers have been widely used in daily life, but most of these materials are easy to burn and often bring safety hazards to people's lives and property

Method used

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  • Flame retardant charring agent-tetra-{1-oxyphospha-2,6,7-trioxabicyclo-[2.2.2]-octane-(4)-methyl} silicate compound and preparation method thereof
  • Flame retardant charring agent-tetra-{1-oxyphospha-2,6,7-trioxabicyclo-[2.2.2]-octane-(4)-methyl} silicate compound and preparation method thereof
  • Flame retardant charring agent-tetra-{1-oxyphospha-2,6,7-trioxabicyclo-[2.2.2]-octane-(4)-methyl} silicate compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1 In a 250ml four-necked flask equipped with a magnetic stirrer, a thermometer, a high-efficiency reflux condenser, and a drying tube at the top of the condenser, the air in the flask was replaced with nitrogen, and 7.20g (O.04mol) ) PEPA and 90ml ethylene glycol dimethyl ether, stir, add 1.70g (1.15ml, 0.01mol) silicon tetrachloride dropwise at 20°C, the temperature of the dropping process is controlled not to be higher than 30°C, after the dropping, the temperature is raised React for 8 hours at 85°C. After the HCl gas is released, add 0.2g of triethylamine, keep it warm and stir for 1 hour, and test the pH of the solution at 5-6 as the end of the reaction; cool, filter with suction, and rinse the filter cake with 20ml of water. After suction filtration and drying, PEPA silicate was obtained with a yield of 77.3% and a decomposition temperature of 280±5°C.

Embodiment 2

[0028] Example 2 In a 250ml four-necked flask equipped with a magnetic stirrer, a thermometer, a high-efficiency reflux condenser, and a drying tube at the top of the condenser, the air in the flask was replaced with nitrogen, and 7.56g (O.042mol) ) PEPA and 70ml acetonitrile, stir, add 1.70g (1.15ml, 0.01mol) silicon tetrachloride dropwise at 20°C, the temperature during the dropping process is controlled not to be higher than 30°C, after the dropping, heat up to 80°C, react 10h, after the HCl gas is released, add 0.25g of triethylamine, keep it warm and stir for 1h, the pH of the detection solution is 5-6 as the end of the reaction; cool, filter with suction, rinse the filter cake with 20ml of water, filter with suction, and dry , The four cage ring silicate PEPA ester was obtained, the yield was 80.5%, and the decomposition temperature was 280±5°C.

Embodiment 3

[0029] Example 3 In a 100ml four-necked flask equipped with a magnetic stirrer, a thermometer, a high-efficiency reflux condenser, and a drying tube at the top of the condenser, the air in the flask was replaced with nitrogen, and 8.10g (0.045mol) was added. PEPA and 60ml dioxane, stir, add 1.70g (1.15ml, 0.01mol) silicon tetrachloride dropwise at 20°C, the temperature during the dropping process is controlled not to be higher than 30°C, after dropping, the temperature is raised to 100°C , React for 6h, after the HCl gas is released, add 0.3g pyridine, keep warm and stir for 1h, the pH of the detection solution is 5-6 as the end of the reaction; cool, filter with suction, rinse the filter cake with 20ml of water, filter with suction, and dry , The four cage ring silicate PEPA ester was obtained, the yield was 94.6%, and the decomposition temperature was 280±5°C.

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Abstract

The invention relates to a flame retardant charring agent-tetra-{1-oxyphospha-2,6,7-trioxabicyclo-[2.2.2]-octane-(4)-methyl} silicate compound and a preparation method thereof. The compound has a structural formula shown in the specification. The preparation method comprises the following steps of dropwise adding silicon tetrachloride into a solution of 1-oxyphospha-4-hydroxymethyl-2,6,7-trioxabicyclo-[2.2.2]-octane (PEPA) and an organic solvent at 20 DEG C, heating to 80-140 DEG C, performing stirring reaction for 4-10 hours, adding a fixed quantity of an acid-binding agent, stirring for 1 hours, and ending the reaction when detecting that the pH value of the solution is 5-6; cooling, performing suction filtration, washing by water, and drying to obtain tetra-{1-oxyphospha-2,6,7-trioxabicyclo-[2.2.2]-octane-(4)-methyl} silicate. The compound is the excellent halogen-free phosphorus-silicon synergistic flame retardant charring agent and can be applied to polyolefin, polyester, polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin and the like, the process is simple, the equipment investment is low, and the industrialized production is easy to realize.

Description

Technical field [0001] The invention relates to a flame-retardant carbon-forming agent tetra-cage silicate PEPA ester compound and a preparation method thereof, and in particular to a flame-retardant carbon-forming agent tetrakis {1-oxyphospha-2,6,7- Trioxabicyclo[2.2.2]octane-(4)-methyl}ester compound and its preparation method. The compound contains phosphorus and silicon dual flame retardant elements and can be used as polyolefin, polyester, polyvinyl chloride, polyurethane , Epoxy resin and unsaturated resin, etc. flame retardant char-forming agent. Background technique [0002] With the development of polymer materials science, plastics, rubbers and fibers have been widely used in daily life, but most of these materials are easy to burn and often bring safety hazards to people's lives and property. Therefore, the research and development of flame retardants and flame retardant polymer materials have attracted people's attention. Due to the improvement of flame retardant re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574C08K5/5435C08L23/12
Inventor 韩志慧董信王彦林
Owner RES INST OF XIANGCHENG SUZHOU UNIV OF SCI & TECH
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