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Preparation of polyphosphate flame retardant having dicyclic phosphoric acid ester structure

A technology of bicyclic phosphate and polyphosphate, which is applied in the fields of chemical instruments and methods, organic chemistry, and compounds of Group 5/15 elements of the periodic table, etc., which can solve the problem of material performance degradation, difficult and durable flame retardancy, and thermal stability Low-level problems, to achieve the effect of good char formation, narrow decomposition range, and good thermal stability

Inactive Publication Date: 2008-12-24
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the commercial organic phosphate flame retardants are mostly viscous liquids, which are highly volatile and have low thermal stability during processing.
During the application process, there are migration and precipitation phenomena, which will reduce the performance of the material, and the flame retardancy is also difficult to last

Method used

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  • Preparation of polyphosphate flame retardant having dicyclic phosphoric acid ester structure
  • Preparation of polyphosphate flame retardant having dicyclic phosphoric acid ester structure
  • Preparation of polyphosphate flame retardant having dicyclic phosphoric acid ester structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Step 1: Add 4.5g (0.025mol) of PEPA, 2.3ml (0.025mol) of phosphorus oxychloride and 20ml of dichloromethane into a three-necked flask equipped with a constant pressure dropping funnel, a stirrer and a thermometer. Stir and slowly add 2.51 g (0.025 mol) triethylamine dropwise, and continue to react for 4 hours after the dropwise addition is completed. After the reaction is completed, the salt is removed by filtration to obtain the reaction intermediate. The intermediate was directly used in the next step of synthesis without further isolation.

[0022] Step 2: Add the intermediate mother liquor and bisphenol S (BPS) 6.25g (0.025mol) into a multi-necked flask equipped with a stirrer, a distillation device and a nitrogen inlet and outlet, heat and stir under a nitrogen flow, and evaporate the solvent, and then Gradually raise the temperature by 25°C / hour, and control the reaction at different temperatures for a certain period of time, until the final reaction temperature ...

Embodiment 2

[0025] Step 1: Add 4.5g (0.025mol) of PEPA, 2.98ml (0.033mol) of phosphorus oxychloride and 20ml of dichloromethane into a three-necked flask equipped with a constant pressure dropping funnel, a stirrer and a thermometer. Stir and slowly add 2.51 g (0.025 mol) triethylamine dropwise, and continue to react for 4 hours after the dropwise addition is completed. After the reaction is completed, the salt is removed by filtration to obtain the reaction intermediate. The intermediate was directly used in the next step of synthesis without further isolation.

[0026] Step 2: Add 9.07g (0.036mol) of the intermediate mother liquor and bisphenol S (BPS) into a multi-necked flask equipped with a stirrer, a distillation device and a nitrogen inlet and outlet, heat and stir under a nitrogen flow, and evaporate the solvent, and then Gradually raise the temperature by 25°C / hour, and control the reaction at different temperatures for a certain period of time, until the final reaction temperat...

Embodiment 3

[0029] Step 1: Add 4.5g (0.025mol) of PEPA, 2.3ml (0.025mol) of phosphorus oxychloride and 20ml of dichloromethane into a three-necked flask equipped with a constant pressure dropping funnel, a stirrer and a thermometer. Stir and slowly add 2.51 g (0.025 mol) of triethylamine dropwise, and continue to react for 1 hour after the dropwise addition is completed. After the reaction is completed, the salt is removed by filtration to obtain the reaction intermediate. The intermediate was directly used in the next step of synthesis without further isolation.

[0030] Step 2: Add the intermediate mother liquor and bisphenol S (BPS) 6.25g (0.025mol) into a multi-necked flask equipped with a stirrer, a distillation device and a nitrogen inlet and outlet, heat and stir under a nitrogen flow, and evaporate the solvent, and then Gradually raise the temperature by 25°C / hour, and control the reaction at different temperatures for a certain period of time, until the final reaction temperatur...

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Abstract

The invention discloses a method for preparing olyphosphate ester flame retardant with a bicyclic phosphate ester structure, which belongs to the polymerization type organophosphorous flame retardant structure and preparation method technical field. The invention is characterized in that: polyphosphate ester provided with a repeating unit structure shown at right is prepared, wherein, Ar is equal to bisphenol A, bisphenol S or hydroquinone. The method has the advantages that: the flame retardant has the characteristics of good heat stability, high decomposition temperature, narrow decomposition intervals, good char-forming property and so on. The method can be used for the flame-retarding modification of materials with higher processing temperature such as polyester, polyamide, polycarbonate, a blend of the polyester, the polyamide and the polycarbonate and so on. The preparation method is simple and easy to control.

Description

technical field [0001] The invention belongs to the technical field of polymeric organic phosphorus flame retardant structure and preparation method thereof. The invention relates to a structure of a polymeric organic phosphorus flame retardant with a bicyclic phosphate structure and a preparation method thereof. Background technique [0002] With the rapid development of synthetic materials, synthetic plastics, rubber, and fibers are more and more used in various sectors of the national economy and people's production and life, but at the same time, fires caused by ignition of high polymers are also Therefore, people have higher and higher requirements for the flame retardant properties of synthetic materials. Especially in the high-tech field, people not only require flame-retardant materials to have satisfactory flame-retardant properties, but also require materials to have good physical and mechanical properties and electrical properties, processing fluidity, easy recyc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/04C07F9/6574C09K21/14C09K21/12C08L85/02
Inventor 郑玉斌闫莉郑楠
Owner DALIAN UNIV OF TECH
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