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Flame-retardant char-forming agent tetracage ring pepa silicate compound and preparation method thereof

Active Publication Date: 2017-04-05
RES INST OF XIANGCHENG SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 char-forming agent tetracage ring pepa silicate compound and preparation method thereof
  • Flame-retardant char-forming agent tetracage ring pepa silicate compound and preparation method thereof
  • Flame-retardant char-forming agent tetracage ring pepa silicate compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1 is equipped with magnetic stirrer, thermometer and high-efficiency reflux condenser, and in the 250ml four-neck flask that drying tube is housed on the condenser, replaces the air in the bottle with nitrogen, adds 7.20g (0.04mol ) PEPA and 90ml of ethylene glycol dimethyl ether, stir, at 20 ℃, dropwise add 1.70g (1.15ml, 0.01mol) silicon tetrachloride, the dropping process control temperature is not higher than 30 ℃, after the drop, the temperature rises to 85°C, react for 8 hours, after the HCl gas is released, add 0.2g of triethylamine, keep stirring for 1 hour, test the solution pH = 5-6 as the reaction end point; cool, filter with suction, rinse the filter cake with 20ml of water, Suction filtration and drying to obtain tetracage ring silicate PEPA ester with a yield of 77.3% and a decomposition temperature of 280±5°C.

Embodiment 2

[0028] Embodiment 2 is equipped with magnetic stirrer, thermometer and high-efficiency reflux condenser, and in the 250ml four-necked flask that drying tube is housed on the condenser, replaces the air in the bottle with nitrogen, adds 7.56g (0.042mol ) PEPA and 70ml of acetonitrile, stirring, at 20°C, dropwise add 1.70g (1.15ml, 0.01mol) silicon tetrachloride, the dropping process control temperature is not higher than 30°C. 10h, after the HCl gas is released, add 0.25g of triethylamine, keep stirring for 1h, test the pH of the solution = 5-6 as the reaction end point; cool, filter with suction, rinse the filter cake with 20ml of water, filter with suction, and dry , to obtain tetracage ring silicate PEPA ester with a yield of 80.5% and a decomposition temperature of 280±5°C.

Embodiment 3

[0029] Example 3 In a 100ml four-neck flask equipped with a magnetic stirrer, a thermometer and a high-efficiency reflux condenser, and a drying tube at the top of the condenser, replace the air in the bottle with nitrogen, and add 8.10g (0.045mol) Stir PEPA and 60ml of dioxane, add 1.70g (1.15ml, 0.01mol) of silicon tetrachloride dropwise at 20°C, control the temperature during the dropwise addition to not higher than 30°C, and raise the temperature to 100°C after dropping , react for 6 hours, after the HCl gas is released, add 0.3g pyridine, keep stirring for 1 hour, test the solution pH = 5-6 as the reaction end point; cool, filter with suction, rinse the filter cake with 20ml of water, filter with suction, and dry , to obtain tetracage ring silicate PEPA ester with a yield of 94.6% and a decomposition temperature of 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 present invention relates to a flame-retardant char-forming agent tetracage ring silicate PEPA ester compound and a preparation method thereof, in particular to a flame-retardant char-forming agent tetra{1-oxyphospha-2,6,7- Trioxabicyclo[2.2.2]octane-(4)-methyl} ester compound and preparation method thereof, the compound contains phosphorus and silicon double flame-retardant elements, and can be used as polyolefin, polyester, polyvinyl chloride, polyurethane , epoxy resin and unsaturated resin flame retardant charcoal agent. Background technique [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. Therefore, the research and development of flame retardants and flame retardant polymer materials has received people's attention. Due to the increasing improvement of flame re...

Claims

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Application Information

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Patent Type & Authority Patents(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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