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Preparation method of DOPO vinylidene bridged derivative, flame retardant and flame-retardant polymer material

A vinylidene bridge chain and derivative technology, applied in the field of flame retardant preparation, can solve the problems of high energy consumption of raw material backflow, difficult to obtain raw materials, low yield and the like

Active Publication Date: 2020-03-17
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The existing DiDOPO preparation method with vinylidene bridge chain structure has the following problems: high preparation cost, low yield, long reaction time, serious backflow of raw materials during the reaction process, large energy consumption, unfriendly preparation process environment, and difficult access to raw materials

Method used

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  • Preparation method of DOPO vinylidene bridged derivative, flame retardant and flame-retardant polymer material
  • Preparation method of DOPO vinylidene bridged derivative, flame retardant and flame-retardant polymer material
  • Preparation method of DOPO vinylidene bridged derivative, flame retardant and flame-retardant polymer material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] Example 1 Preparation of DOPO Bridged Derivatives of Formula (V) [6H-Dibenzo[c,e][1,2]Oxophosphoglyceride, 6,6'-(1,2-Ethylenediyl) bis-,6,6'-dioxide]

[0071] DOPO32.4g (0.15mol), diphenylmethane 25g and 20g xylene were added to a four-necked flask equipped with a thermometer, a water separator, a mechanical stirrer and a constant pressure funnel.

[0072] Under the protection of nitrogen, the mixed solution was heated to 195° C., and 6.6 g (0.075 mol) of ethylene carbonate was started to be added dropwise at a constant speed. After 1 hour, the result of sampling and measuring the nuclear magnetic phosphorus spectrum showed that the crude yield of the product was only 1.8%, and the reaction was completed at this speed. 40 hours or more.

[0073] Therefore, add 0.34g (0.0023mol) sodium iodide to the 4.5g ethylene carbonate that has not been added dropwise and continue to drop after mixing uniformly, dropwise in 1.5 hours, and continue to insulate for 2.5 hours to comple...

Embodiment 2

[0078] Example 2 Preparation of DOPO Bridged Derivatives of Formula (V) [6H-Dibenzo[c,e][1,2]Oxophosphoglyceride, 6,6'-(1,2-Ethylenediyl) bis-,6,6'-dioxide]

[0079] DOPO32.4g (0.15mol), 25g diphenylmethane and 20g xylene were added to a four-neck flask equipped with a thermometer, a water separator, a mechanical stirrer and a constant pressure funnel.

[0080] Under nitrogen protection, the mixed solution was heated to 195° C., and a mixed solution of 0.34 g (0.0023 mol) sodium iodide and 6.6 g (0.075 mol) ethylene carbonate was added dropwise, and the dropwise addition was completed within 2.5 hours. A large amount of gas was generated from the bubbler of the tail gas, the reflux of the reaction system was not serious, and the reaction temperature was kept stably at 195°C. After 2 hours of incubation, the reaction was terminated.

[0081] After cooling, add 38g of isopropanol and stir under reflux for 20 minutes, the system is white and turbid. After cooling, the solid pr...

Embodiment 3

[0082] Example 3 Preparation of DOPO Bridged Derivatives of Formula (V) [6H-Dibenzo[c,e][1,2]Oxophosphoglyceride, 6,6'-(1,2-Ethylenediyl) bis-,6,6'-dioxide]

[0083] DOPO38.9g (0.18mol) and 20g xylene were added to a four-necked flask equipped with a thermometer, a water separator, a mechanical stirrer and a constant pressure funnel.

[0084] Under the protection of nitrogen, the mixed solution was heated to 195°C, and the mixed solution of 0.27g (0.0018mol) sodium iodide and 5.28g (0.06mol) ethylene carbonate was added dropwise, and the dropwise addition was completed within 2 hours, and then the insulation was continued for 2.5 hours. The reaction is over.

[0085] After cooling, add 40g of isopropanol and stir under reflux for 20 minutes, the system is white and turbid. Suction filtration after standing to cool, the solid product was first washed with isopropanol, then washed three times with an appropriate amount of deionized water, and after vacuum drying at 180 ° C, 20.8...

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Abstract

The invention discloses a preparation method of a DOPO vinylidene bridged derivative, a flame retardant and a flame-retardant polymer material. The method is characterized in that a DOPO compound reacts with cyclic carbonate in a reaction system containing the DOPO compound and cyclic carbonate to obtain the DOPO vinylidene bridged derivative. The method can be used for efficiently, simply and conveniently preparing the DOPO vinylidene bridged derivative with low energy consumption. The invention also provides the flame retardant containing the product prepared by the method and the flame-retardant polymer material containing the product prepared by the method.

Description

technical field [0001] The invention relates to a preparation method of DOPO vinylidene bridge chain derivatives, a flame retardant and a flame retardant polymer material, belonging to the field of flame retardant preparation. Background technique [0002] Polymer materials are widely used in electronic appliances, automobiles, construction, textiles and other industries. However, due to the flammability of polymer materials, it is necessary to add flame retardants in actual use to meet the requirements of fire safety. Phosphonate esters, especially 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) bridge chain derivative flame retardants have received attention due to their high flame retardant efficiency and environmental friendliness. [0003] US Patent No. 9522927 reports DiDOPO with vinylidene bridge chain structure. The preparation process uses DOPO, dichloroethane and expensive strong base as reactants, and the yield is low and the cost is high. [0004] U.S...

Claims

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Application Information

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IPC IPC(8): C07F9/6571C08K5/5313
CPCC07F9/657172C08K5/5313C07F9/6571
Inventor 姚强赵月英曹微虹唐天波
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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