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, s

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
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Example Embodiment

[0070] Example 1 Preparation of DOPO bridged chain derivative of formula (V) [6H-dibenzo[c,e][1,2]oxophosphoglyceride, 6,6'-(1,2-ethylenediyl) Bis-,6,6'-dioxide]

[0071] 32.4 g (0.15 mol) of DOPO, 25 g of diphenylmethane and 20 g of xylene were added to a four-necked flask equipped with a thermometer, a water trap, a mechanical stirring and a constant pressure funnel.

[0072] Under the protection of nitrogen, the mixture was heated to 195°C, and 6.6 g (0.075 mol) of ethylene carbonate was added dropwise at a uniform rate. After 1 hour, a sample was taken to measure the NMR spectrum and the results showed that the crude yield of the product was only 1.8%. The reaction was completed at this speed. More than 40 hours.

[0073] Therefore, 0.34 g (0.0023 mol) of sodium iodide was added to the 4.5 g of ethylene carbonate that had not been dripped and mixed uniformly, and then the dripping was continued. After 1.5 hours of dripping, the reaction was completed after the temperature was ke...

Example Embodiment

[0078] Example 2 Preparation of DOPO bridged chain derivative of formula (V) [6H-dibenzo[c,e][1,2]oxophosphoglyceride, 6,6'-(1,2-ethylenediyl) Bis-,6,6'-dioxide]

[0079] 32.4 g (0.15 mol) of DOPO, 25 g of diphenylmethane and 20 g of xylene were added to a four-necked flask equipped with a thermometer, water trap, mechanical stirring and a constant pressure funnel.

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

[0081] Cool, add 38 g of isopropanol, stir under reflux for 20 minutes, the system is white turbid. After standing to cool and...

Example Embodiment

[0082] Example 3 Preparation of DOPO bridged chain derivative of formula (V) [6H-dibenzo[c,e][1,2]oxophosphoglyceride, 6,6'-(1,2-ethanediyl) Bis-,6,6'-dioxide]

[0083] 38.9 g (0.18 mol) of DOPO and 20 g of xylene were added to a four-necked flask equipped with a thermometer, water separator, mechanical stirring 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. The addition was completed within 2 hours, and the temperature was kept for 2.5 hours. The reaction is over.

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

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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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