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Melamine polyphosphoric acid rare earth metal salt, synthetic method and application

A technology of rare earth and rare earth metal salts of melamine polyphosphate, which is applied in the direction of organic chemistry, can solve the problems of environmental protection and hygienic restrictions, and achieve the effects of improving thermal stability, high flame retardant efficiency, and simple synthesis process

Inactive Publication Date: 2015-11-11
广东华南精细化工研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The representative products of organic flame retardants are halogenated flame retardants, especially brominated flame retardants, which have good flame retardant cost performance and are the most widely used flame retardants in the market, but their environmental protection and hygiene Controversy limits its further use

Method used

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  • Melamine polyphosphoric acid rare earth metal salt, synthetic method and application
  • Melamine polyphosphoric acid rare earth metal salt, synthetic method and application
  • Melamine polyphosphoric acid rare earth metal salt, synthetic method and application

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Experimental program
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Effect test

Embodiment 1 3

[0041] Embodiment 1 Melamine polyphosphate lanthanum salt

[0042] 12.5g of melamine and 9.9g of lanthanum oxide were added to a 500ml four-neck flask filled with 300ml of distilled water, a stirring bar and a thermometer, and the temperature was slowly raised to 80°C under stirring, and 4.6g of hydrochloric acid (37%wt) was added dropwise to the flask, measured The pH value of the solution was about 6.0. After stirring for 1.0 h, 22.2 g of sodium pyrophosphate was added. After reacting for 1 h at 80° C., 16.5 g of hydrochloric acid (37% wt) was added dropwise to the flask for the second time, and the pH value of the solution was measured to be about 6.0. 2.0, continue to react for 1.0 h, cool to room temperature, filter, centrifuge, wash with distilled water until neutral, and dry to obtain lanthanum melamine polyphosphate with a yield of 83%. After elemental analysis, the content of lanthanum element was 13.5%.

Embodiment 2 3

[0043] Embodiment 2 Melamine polyphosphate cerium salt

[0044] 12.5g of melamine and 9.7g of cerium chloride were added to a 500ml four-neck flask filled with 300ml of distilled water, a stirring bar and a thermometer, and the temperature was slowly raised to 90°C under stirring, and 4.8g of hydrochloric acid (37%wt) was added dropwise to the flask. The pH value of the solution was measured to be about 5.0. After stirring for 0.5 h, 22.2 g of sodium pyrophosphate was added. After reacting for 0.5 h at 90° C., 16.5 g of hydrochloric acid (37% wt) was added dropwise to the flask for the second time, and the pH of the solution was measured. The value is about 2.0, continue to react for 1.5h, cool to room temperature, filter, centrifuge, wash with distilled water until neutral, and dry to obtain cerium melamine polyphosphate with a yield of 85%. According to elemental analysis, the content of cerium element is 13.4%.

Embodiment 3 3

[0045] Embodiment 3 melamine polyphosphate praseodymium salt

[0046] 12.5g of melamine and 5.9g of praseodymium hydroxide were added to a 500ml four-neck flask filled with 300ml of distilled water, a stirring bar and a thermometer, and the temperature was slowly raised to 90°C under stirring, and 4.6g of hydrochloric acid (37%wt) was added dropwise to the flask. The pH value of the solution was measured to be about 6.0. After stirring for 0.5 h, 22.2 g of sodium pyrophosphate was added. After reacting for 0.5 h at 90° C., 16.3 g of hydrochloric acid (37% wt) was added dropwise to the flask for the second time, and the pH of the solution was measured. The value was about 3.0, continued to react for 1.5h, cooled to room temperature, filtered, centrifuged, washed with distilled water until neutral, and dried to obtain praseodymium melamine polyphosphate with a yield of 86%. According to elemental analysis, the content of praseodymium element is 13.0%.

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Abstract

Melamine polyphosphoric acid rare earth metal salt, a synthetic method and application belong to the field of chemical synthesis. According to the invention, by combining stable melamine polyphosphoric acid with light rare earth elements with unique electron distribution and corresponding electron cloud density, a dual effect of being good in thermal stability, high in phosphorus content and high in char forming catalytic efficiency and improving compatibility and flame-retardant synergistic effect by rare earth coordinate bonding is fully exerted, and the melamine polyphosphoric acid rare earth metal salt can be applied to an intumescent flame-retardant system. The chemical synthetic method comprises a solution method and a calcining method. The formula is shown in the description, wherein M is a rare earth element in lanthanide series, n1 is an integer which is greater than or equal to 2 and n2 is an integer of 1, 2 or 3.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and relates to a phosphorus-nitrogen synergistic flame-retardant halogen-free rare earth compound and a preparation process thereof, in particular to a melamine polyphosphate rare earth metal salt and a preparation method thereof. The compound can be used as polyester, polyamide Flame retardant application of macromolecule materials such as class and oxygen-containing resin. Background technique [0002] Development of Phosphorous Flame Retardants. [0003] With the successive implementation of domestic and foreign environmental protection regulations, the replacement of halogenated flame retardants is becoming more and more urgent. Phosphorus-based flame retardants are most likely to become the next-generation mainstream flame retardants due to their characteristics in terms of the balance of flame retardant performance and physical and mechanical properties, product variety, and product appli...

Claims

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Application Information

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IPC IPC(8): C07D251/56C08K5/3492C08L67/02
CPCC07D251/56C08K5/34928C08L2201/02
Inventor 王朝晖陈宇赵欣刘火钦汤永华
Owner 广东华南精细化工研究院有限公司
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