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Method for preparing high-purity pyrophosphoric acid amine salt

A pyrophosphate amine salt, pyrophosphate technology, applied in the preparation of organic compounds, the preparation of amino compounds, chemical instruments and methods, etc., can solve the problems of reducing flame retardant performance, multiple impurities, expensive raw materials, etc., to achieve flame retardant Improved performance, high degree of mixing, and improved purity

Active Publication Date: 2014-12-24
PRESAFER QINGYUAN PHOSPHOR CHEM
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  • Description
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Problems solved by technology

[0003] For example, German Patent DE-A-10145093, European Patent EP-A-1277794, etc. disclose a variety of methods for preparing ammonium pyrophosphate, but the yield of the corresponding ammonium pyrophosphate produced by the above method is extremely low, and Contains more impurities, which reduces its flame retardant performance; due to the low yield of the above-mentioned preparation method, the raw material is expensive, and the product is difficult to purify, the use of the above-mentioned method is limited.

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  • Method for preparing high-purity pyrophosphoric acid amine salt

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preparation example Construction

[0023] A preparation method of high-purity ammonium pyrophosphate, comprising the following steps:

[0024] 1) Prepare the mixture by one of the following three methods:

[0025] A: Disperse pyrophosphate in water, add acid while stirring, control the reaction temperature at 0-100°C (preferably, the reaction temperature is controlled at 3-10°C), and the reaction time is 0.1-2h; in the above reaction solution Add one or more amine substances, and add an adsorbent at the same time, control the reaction temperature at 0-100°C, and react for 0.5-5h to obtain a mixed solution;

[0026] B: Disperse one or more amine substances in water, add acid while stirring, control the reaction temperature at 0-100°C (preferably, the reaction temperature is controlled at 3-10°C), and the reaction time is 0.1-2h; Add pyrophosphate to the above reaction solution, and add an adsorbent at the same time, control the reaction temperature at 0-100°C, and react for 0.5-5 hours to obtain a mixed solutio...

Embodiment 1

[0048] 1) In a 500L reactor with a stirring and condensing device, disperse 81.36kg of anhydrous sodium pyrophosphate in 300L of pure water, add 123.02kg of hydrochloric acid with a mass concentration of 36%, control the reaction temperature at 5°C, and the reaction time After 1.5 hours, the mixture was obtained;

[0049] 2) Add 26.97kg of tetramethylenediamine and 1.0kg of modified zeolite particles to the above mixed solution in sequence (the preparation method of modified zeolite is: zeolite (particle size: 3-20mm) soaked in 10wt% NaOH solution for 6 hours , washed and dried, and then saturated NaCl solution at room temperature (saturated NaCl solution at room temperature can also be replaced with 5wt% FeCl 3 solution, or saturated CaCl at room temperature 2 solution) soaked for 24 hours, washed and dried to obtain modified zeolite), the reaction temperature was controlled at 5°C, and the reaction time was 3 hours;

[0050] 3) When discharging the above mixture, add a sie...

Embodiment 2

[0055] 1) In a 500L reactor with a stirring and condensing device, disperse 81.36kg of anhydrous sodium pyrophosphate in 300L of pure water, add 123.02kg of hydrochloric acid with a mass concentration of 36%, control the reaction temperature at 5°C, and the reaction time After 1.5 hours, the mixture was obtained;

[0056]2) Add 22.68kg of 1,3-propylenediamine and 1.5kg of activated carbon loaded with zirconia to the above mixture in sequence (the preparation method is: soak activated carbon (particle size: 3-20mm) in 10wt% NaOH solution for 24 hours, pump Filter, wash with deionized water until neutral, dry, soak in 20wt% hydrochloric acid for 12 hours, filter with suction, wash with deionized water until neutral, dry, place the dried activated carbon in a zirconium concentration of 0.5mol / Immerse in an aqueous solution of L zirconium oxychloride for 24 hours, filter with suction, wash with deionized water for several times until no chloride ions are detected, and solidify th...

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Abstract

The invention discloses a method for preparing a high-purity pyrophosphoric acid amine salt. The method comprises the following steps: 1) preparing a mixture liquid by using one of the three methods: A, dispersing pyrophosphate in water, adding acid to react, further adding an amine substance and an absorbent, and reacting so as to obtain the mixture liquid; B, dispersing one or more amine substances into water, adding acid to react, further adding pyrophosphate and the absorbent, and reacting so as to obtain the mixture liquid; C, dispersing pyrophosphate and one or more amine substances into water to react, further adding acid and the absorbent, and reacting so as to obtain the mixture liquid; 2) removing the absorbent in the mixture liquid, separating the liquid from a solid, putting the obtained solid into an EDTA (Ethylene Diamine Tetraacetic Acid) water solution, sufficiently stirring and mixing, further separating the liquid from the solid, washing by using water, and further washing by using ethanol; 3) drying the washed solid so as to obtain the high-purity pyrophosphoric acid amine salt. The method is high in yield, and the obtained pyrophosphoric acid amine salt is high in purity and good in flame retardation property.

Description

technical field [0001] The invention relates to a preparation method of high-purity ammonium pyrophosphate. Background technique [0002] Ammonium pyrophosphate, as an important component (carbon source, gas source, etc.) of halogen-free intumescent flame retardants, has excellent flame retardant effect, and has attracted more and more attention from the flame retardant industry. For the preparation method of amine pyrophosphate, many proposals have been proposed. [0003] For example, German Patent DE-A-10145093, European Patent EP-A-1277794, etc. disclose a variety of methods for preparing ammonium pyrophosphate, but the yield of the corresponding ammonium pyrophosphate produced by the above method is extremely low, and Contains more impurities, which reduces its flame retardant performance; due to the low yield of the above-mentioned preparation method, the raw material is expensive, and the product is difficult to purify, the use of the above-mentioned method is limited...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/09C07C211/11C07C209/00C08K5/17C08K5/3492C08L23/14
Inventor 黄超陈志钊周侃
Owner PRESAFER QINGYUAN PHOSPHOR CHEM
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