Preparation method of reactive nitrogen-phosphorus flame retardant for aqueous polyurethane

A nitrogen-phosphorus flame retardant, water-based polyurethane technology, applied in the field of flame retardant modified polyurethane flame retardant, can solve the problems of reducing flame retardancy and being susceptible to heat precipitation, and achieves good flame retardant effect, high synthesis efficiency, and structure. stable effect

Active Publication Date: 2019-01-11
SICHUAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, small molecular nitrogen and phosphorus flame retardants are easy to be ...

Method used

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  • Preparation method of reactive nitrogen-phosphorus flame retardant for aqueous polyurethane
  • Preparation method of reactive nitrogen-phosphorus flame retardant for aqueous polyurethane
  • Preparation method of reactive nitrogen-phosphorus flame retardant for aqueous polyurethane

Examples

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Effect test

Embodiment 1

[0026] The steps of this embodiment are as follows:

[0027] (1) Preparation of phosphorus-containing derivatives

[0028] Add 9,10-dihydro-9-oxa-10-phospha-phenanthrene-10-oxide (DOPO), 2-butene-1,4-dioic acid and solvent propionic acid into the reaction vessel and mix well, Addition reaction was then carried out under stirring at 140°C for 12h. After the reaction time was up, the reaction mixture was vacuum-dried at a vacuum degree of 0.085MPa and a temperature of 40°C for 10h to obtain a phosphorus-containing derivative. The 9, The molar ratio of 10-dihydro-9-oxa-10-phospha-phenanthrene-10-oxide, 2-butene-1,4-dioic acid and propionic acid is 1:1:20;

[0029] (2) Preparation of reactive nitrogen and phosphorus flame retardants

[0030] The phosphorus-containing derivative obtained in step (1), N,N-bis(2-hydroxyethyl)aminomethylene phosphonic acid diethyl ester (FRC-6), water-carrying agent toluene and catalyst p-toluenesulfonic acid Add it into the reaction container and ...

Embodiment 2

[0040] The steps of this embodiment are as follows:

[0041] (1) Preparation of phosphorus-containing derivatives

[0042] Add 9,10-dihydro-9-oxa-10-phospha-phenanthrene-10-oxide (DOPO), 2-propylene-1,2-dicarboxylic acid and solvent butanoic acid to the reaction vessel and mix uniform, and then add reaction at 180°C for 24 hours under stirring. After the reaction time is up, the reaction mixture is vacuum-dried at a vacuum degree of 0.095MPa and a temperature of 60°C for 24 hours to obtain a phosphorus-containing derivative. The molar ratio of 9,10-dihydro-9-oxa-10-phospha-phenanthrene-10-oxide, 2-propylene-1,2-dicarboxylic acid and butyric acid is 1:3:100;

[0043] (2) Preparation of reactive nitrogen and phosphorus flame retardants

[0044] Add phosphorus-containing derivatives obtained in step (1), N,N-bis(2-hydroxyethyl)aminomethylenephosphonic acid diethyl ester (FRC-6), water-carrying agent xylene and catalyst thionyl chloride Mix evenly in the reaction container, and...

Embodiment 3

[0047] The steps of this embodiment are as follows:

[0048] (1) Preparation of phosphorus-containing derivatives

[0049] Add 9,10-dihydro-9-oxa-10-phospha-phenanthrene-10-oxide (DOPO), 2-methyl-2,5-furandione and solvent benzene into the reaction vessel and mix well, Addition reaction was then carried out under stirring at 160°C for 16h. After the reaction time was up, the reaction mixture was vacuum-dried for 20h at a vacuum degree of 0.090MPa and a temperature of 50°C to obtain a phosphorus-containing derivative. The 9, The molar ratio of 10-dihydro-9-oxa-10-phospha-phenanthrene-10-oxide, 2-methyl-2,5-furandione and benzene is 1:2:80;

[0050] (2) Preparation of reactive nitrogen and phosphorus flame retardants

[0051] With step (1) gained phosphorus-containing derivative, N,N-bis(2-hydroxyethyl)aminomethylene phosphonic acid diethyl ester (FRC-6), water-carrying agent ethylbenzene and catalyst concentrated hydrochloric acid (mass concentration greater than 20%) into t...

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Abstract

The invention relates to a preparation method of a reactive nitrogen-phosphorus flame retardant for aqueous polyurethane. The preparation method comprises: (1) adding 9,10-dihydro-9-oxa-10-phospha-phenanthrene-10-oxide, a dicarboxylic acid with a double bond or an anhydride with a double bond, and a solvent A to a reaction container, uniformly mixing, carrying out an addition reaction for 12-24 hat a temperature of 140-180 DEG C under stirring, and carrying out vacuum drying on the mixture obtained by the reaction after achieving the reaction time to obtain a phosphorus-containing derivative;and (2) adding the phosphorus-containing derivative obtained in the step (1), diethyl bis(2-hydroxyethyl)aminomethylphosphonate, a water-carrying agent B and a catalyst C to a reaction container, mixing uniformly, carrying out an esterification reaction for 12-24 h at a temperature of 140-160 DEG C under stirring, and carrying out vacuum drying on the mixture obtained by the reaction after achieving the reaction time to obtain the reactive nitrogen-phosphorus flame retardant. According to the present invention, the reactive nitrogen-phosphorus flame retardant for aqueous polyurethane is prepared by the above method.

Description

technical field [0001] The invention belongs to the field of flame retardants for polyurethane flame retardant modification, and relates to a halogen-free flame retardant for waterborne polyurethane flame retardant modification and a preparation method thereof. technical background [0002] As an environment-friendly polymer material with excellent processability and low VOCs, waterborne polyurethane (WPU) has received extensive attention and research. However, due to its inherent flammability, the application of WPU in products such as leather, textiles, films and adhesives is greatly limited. Therefore, in order to broaden the application fields of WPU, it is urgent to improve the flame retardancy of WPU. [0003] In the past few decades, halogenated flame retardants (especially brominated flame retardants) have been widely used in the flame retardant modification of polyurethane. However, brominated flame retardants release a large amount of toxic gases and corrosive fu...

Claims

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Application Information

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IPC IPC(8): C08G63/692C08G18/46
Inventor 杜晓声王双成煦杜宗良王海波
Owner SICHUAN UNIV
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