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Buckling flame retardant containing phosphor-nitrogen macromolecule and preparation method thereof

An intumescent flame retardant and macromolecular technology, applied in fire-resistant coatings and other directions, can solve the problems of easy migration or precipitation, loss of flame retardant performance, small molecular weight, etc., and achieve good application prospects, easy control, and simple preparation methods. Effect

Inactive Publication Date: 2008-07-23
NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There have been many patent reports related to the types of phosphorus-nitrogen series intumescent flame retardants, mainly including the single-component pentaerythritol phosphate melamine salt, and the three-component ammonium polyphosphate / pentaerythritol / melamine intumescent flame retardant. Both one-component and three-component intumescent flame retardants have several disadvantages: one is that the single-component salts are mainly synthesized in water, and the yield is low; the other is that one or several of the main components have different molecular weights. Large, easy to migrate or precipitate when processing with the substrate, resulting in loss of flame retardant properties

Method used

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  • Buckling flame retardant containing phosphor-nitrogen macromolecule and preparation method thereof
  • Buckling flame retardant containing phosphor-nitrogen macromolecule and preparation method thereof
  • Buckling flame retardant containing phosphor-nitrogen macromolecule and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Under nitrogen protection, 59.4g of 2,6,7-trioxo-1-phosphabicyclo-[2,2,2]-octane-1-methoxy dichlorophosphate was dissolved in 100ml of acetonitrile In a 250ml three-neck flask, heat while stirring. After the dissolution is complete, start to drop 40g of 4,4'-diaminodiphenylmethane in acetonitrile solution. After the dropwise addition, start to drop 15ml of catalyst pyridine. During the reaction, light yellow powder was continuously generated, reacted for 5 hours, filtered, washed twice with deionized water, and then washed twice with absolute ethanol. Dry in a vacuum oven at 80° C. for 12 hours to obtain a light yellow powder solid with a yield of 85%. Melting point 255-258°C, elemental analysis: C%: 48.1%, H%: 5.0%, N%: 4.83%, O%: 25.8%, P%: 16.27%. See Figure 1 for the NMR spectrum. The result proves that the compound synthesized by the preparation method of the present invention is basically consistent with the designed phosphorus- and nitrogen-containing macromole...

Embodiment 2

[0030] Under nitrogen protection, 29.7g of 2,6,7-trioxo-1-phosphabicyclo-[2,2,2]-octane-1-methoxy dichlorophosphate was dissolved in 80ml of acetonitrile In a 250ml three-neck flask, heat while stirring, and after it dissolves, start to drop 20g of 4,4'-diaminodiphenylmethane in acetonitrile solution, after the dropwise addition, start to drop 10ml of catalyst pyridine, at 80°C During the reaction, light yellow powder was continuously generated. After 2 hours of reaction, it was filtered, and the filter cake was washed twice with deionized water and then twice with absolute ethanol. After drying in a vacuum oven at 80°C for 12 hours, a light yellow powder solid was obtained with a yield of 75%. Melting point 255-257°C, elemental analysis: C%: 46.2%, H%: 4.8%, N%: 5.85%, O%: 25.9%, P%: 17.25%.

Embodiment 3

[0032] Under nitrogen protection, 59.4g of 2,6,7-trioxo-1-phosphabicyclo-[2,2,2]-octane-1-methoxy dichlorophosphate was dissolved in 120ml of acetonitrile In a 250ml three-neck flask, heat while stirring. After the dissolution is complete, start to drop 42g of 4,4'-diaminodiphenylsulfone in acetonitrile solution. After the dropwise addition, start to add 20ml of catalyst pyridine dropwise. During the reaction, light yellow powder was continuously generated, reacted for 4 hours, filtered, washed twice with deionized water, and then washed twice with absolute ethanol. Dry in a vacuum oven at 80° C. for 12 hours to obtain a light yellow powder solid with a yield of 78%. Melting point 256-258°C, elemental analysis: C%: 43.6%, H%: 4.1%, N%: 5.23%, O%: 26.9%, P%: 16.77%, S%: 3.4%.

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Abstract

The invention relates to a macromolecular intumescent flame retardant with phosphorus and nitrogen, which is characterized in that: the chemical composition is poly (2, 6 and 7-trioxy-1-phosphorous dicyclic-[2, 2 and 2]-octane-1-anisyl) organic phosphate 4 and 4'-diaminodiphenylmethane; the preparation process is that: 2, 6 and 7-trioxy-1-phosphorous dicyclic-[2, 2 and 2]-octane-1-anisyl is put into the solvent of acetonitrile and dissolved after heating and stirring, and then diamine compound and catalyst are added into the solution, and a temperature reaction is processed under the protection of nitrogen; the solution is filtered when reaction is over to obtain the filter mass after being rinsed and dried. The macromolecular intumescent flame retardant with phosphorus and nitrogen has the advantages of being halogen-free and environment-friendly, big molecular weight, basically solving transplantation, separation, volatilization or other problems on the machineshaping of the flame retardant and the polymer substrate, simple preparation method and operation and higher productive rate of the product.

Description

technical field [0001] The invention relates to a phosphorus- and nitrogen-containing macromolecular expansion type flame retardant, and the invention also relates to a preparation method of a phosphorus- and nitrogen-containing macromolecular expansion type flame retardant. Background technique [0002] Intumescent flame retardant (IFR) is a flame retardant with phosphorus, nitrogen and carbon as the main core elements. This type of flame retardant is specially developed for the flame retardancy of polyolefins and shows excellent flame retardancy. This type of flame retardant has become a new type of environmentally friendly flame retardant that can replace halogen-containing flame retardants due to its good flame retardant performance. According to the number of flame retardant components, it is generally divided into single-component and multi-component (mixed) intumescent flame retardants. [0003] There have been many patent reports related to the types of phosphorus-n...

Claims

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Application Information

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IPC IPC(8): C09K21/14C08G79/02C08L23/00
Inventor 方征平宋平安郭正虹
Owner NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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