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Cage-shaped flame-retardant charring agent trimethyl silicic acid PEPA ester compound and preparation method thereof

A technology of trimethylsilicate and ester compounds, applied in chemical instruments and methods, compounds of group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problems of secondary combustion of materials and achieve good char formation , simple equipment and low cost

Inactive Publication Date: 2014-08-27
SHANDONG XINGQIANG CHEM IND TECH RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Generally, the addition of flame retardants to polymer materials can prevent the combustion of materials, but at high temperatures, materials tend to melt and drip when heated, resulting in secondary combustion

Method used

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  • Cage-shaped flame-retardant charring agent trimethyl silicic acid PEPA ester compound and preparation method thereof
  • Cage-shaped flame-retardant charring agent trimethyl silicic acid PEPA ester compound and preparation method thereof
  • Cage-shaped flame-retardant charring agent trimethyl silicic acid PEPA ester compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1 is equipped with magnetic stirrer, thermometer and high-efficiency reflux condenser, and in the 100ml four-neck flask that drying tube is housed on the condenser upper mouth, replace the air in the bottle with nitrogen, 4.5g (0.025mol) Add PEPA and 30ml of ethylene glycol dimethyl ether into the four-necked flask, stir, and drop 2.716g (3.17ml, 0.025mol) trimethylchlorosilane into the four-necked flask at 50°C, and control the temperature during the dropping process. When the temperature is higher than 60°C, after dropping, raise the temperature to 85°C, and react for 10 hours. After the HCl gas is released, add 0.15 g of triethylamine, keep stirring for 1 hour, and detect the pH of the solution = 5-6 as the reaction end point. The solvent is recovered by distillation under reduced pressure, and the solid crude product is left in the retort, converted into a reflux device, and then added with 30ml of absolute ethanol, stirred and heated to dissolve, cooled, ...

Embodiment 2

[0029] Embodiment 2 is equipped with magnetic stirrer, thermometer and high-efficiency reflux condenser, and in the 100ml four-neck flask that drying tube is housed on the condenser, replace the air in the bottle with nitrogen, and 4.5g (0.025mol) Add PEPA and 20ml of acetonitrile into the four-necked flask, stir, and drop 2.99g (3.48ml, 0.0275mol) trimethylchlorosilane into the four-necked flask at 50°C. After dropping, raise the temperature to 80°C and react for 11 hours. After the HCl gas is released, add 0.2 g of pyridine and keep stirring for 1 hour. The pH of the solution is detected to be 5-6 as the reaction end point. The solvent is recovered by distillation under reduced pressure, and the solid crude product is left in the retort, converted into a reflux device, and then added with 30ml of absolute ethanol, stirred and heated to dissolve, cooled, and the product is fully crystallized, filtered, and dried to obtain a cage The flame retardant char-forming agent PEPA tri...

Embodiment 3

[0030] Embodiment 3 is equipped with magnetic stirrer, thermometer and high-efficiency reflux condensation tube, and in the 100ml four-neck flask that drying tube is housed on the top of condensation tube, replace the air in the bottle with nitrogen, and 4.5g (0.025mol) Add PEPA and 50ml of dioxane into the four-necked flask, stir, and drop 3.26g (3.80ml, 0.03mol) trimethylchlorosilane into the four-necked flask at 50°C, the dropping process controls the temperature not higher than 60°C, after dripping, raise the temperature to 100°C, react for 8 hours, after the HCl gas is released, add 0.25g pyridine, keep stirring for 1 hour, and detect the pH of the solution = 5-6 as the reaction end point. The solvent is recovered by distillation under reduced pressure, and the solid crude product is left in the retort, converted into a reflux device, and then added with 30ml of absolute ethanol, stirred and heated to dissolve, cooled, and the product is fully crystallized, filtered, and d...

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Abstract

The invention relates to a cage-shaped flame-retardant charring agent trimethyl silicic acid PEPA ester compound and a preparation method of the cage-shaped flame-retardant charring agent trimethyl silicic acid PEPA ester compound. The structure of the compound is shown through the following formula in the specification. The preparation method includes the steps that at the temperature of 50 DEG C, trimethylchlorosilane is dripped to a solution of 1-epoxide phosphole -4-hydroxymethyl-2, 6, 7-trioxa-bicyclo [2.2.2] octane (PEPA) and an organic solvent, the temperature rises to 80 DEG C to 140 DEG C, a reaction is conducted for 5 h to 11 h through stirring, a quantitative acid-binding agent is added, stirring is conducted for 1 h, when the pH of the solution is detected as 5 to 6, the reaction is ended, after reduced pressure distillation, purification treatment is conducted, and then cage-shaped flame-retardant charring agent trimethyl silicic acid PEPA ester is acquired. The compound is an excellent halogen-free phosphorus and silicon synergistic flame-retardant charring agent, can be applied to polyolefin, polyester, polyvinyl chloride, polyurethane, epoxy resin, unsaturated polyester resin and the like, and is simple in process and small in equipment investment, and industrial production can be easily achieved.

Description

technical field [0001] The invention relates to a cage-shaped flame-retardant char-forming agent trimethylsilicate PEPA compound and a preparation method thereof, in particular to a flame-retardant char-forming agent 1-oxyphospha-4-trimethylsiloxymethyl -2,6,7-trioxabicyclo[2.2.2]octane compound and its preparation method, the compound contains phosphorus and silicon double flame retardant elements, and can be used as polyolefin, polyester, polyvinyl chloride, polyurethane, Flame retardant char forming agent for epoxy resin and unsaturated resin. Background technique [0002] With the rapid development of international science, technology and economy, flame retardant materials have developed rapidly. At the same time, due to the enhancement of environmental safety awareness, higher requirements have been put forward for flame retardants. Flame retardant materials are required to be friendly to the environment, so the non-halogenation of flame retardants has become a hot spo...

Claims

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Application Information

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IPC IPC(8): C07F9/6574C08K5/5435C08L23/12
Inventor 韩志慧董信王彦林
Owner SHANDONG XINGQIANG CHEM IND TECH RES INST CO LTD
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