Crystalline aluminum phosphite, and preparation method and application thereof

A technology of aluminum phosphite and aluminum hydrogen phosphite, applied in the field of materials, can solve the problems of easy discoloration, negative impact, easy moisture absorption of flame retardants, etc., and achieve the effects of low water absorption, acidity, and high thermal decomposition temperature

Active Publication Date: 2021-10-01
JIANGSU LISIDE NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the aluminum phosphite reported at present is all non-crystalline compounds, shows certain solubility on physical property, still has certain water absorption and acidity, so in this composite system, still there are several problems: 1) aluminum phosphite There is a certain solubility, so the flame retardant is easy to absorb moisture, and there is a risk of moisture absorption when applied to polymer products, which affects the electrical insulation performance; 2) The certain acidity shown by aluminum phosphite still has certain influence on polymers and processing equipment. Negative impact; 3) The thermal decomposition temperature is slightly insufficient, especially under high shear conditions, such as high glass fiber content, due to the enhanced shear force, the system is easy to change color
These deficiencies limit the scope of application of the flame retardant system

Method used

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  • Crystalline aluminum phosphite, and preparation method and application thereof
  • Crystalline aluminum phosphite, and preparation method and application thereof
  • Crystalline aluminum phosphite, and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0074] The preparation of embodiment 1 crystalline aluminum phosphite

[0075] The preparation process is: add 270g (1mol) aluminum hydrogen phosphite ((H 2 PO 3 ) 3 Al) and the water of 630g, fully stirring and dissolving, obtain aluminum hydrogen phosphite solution. In a 500mL beaker, 75g of aluminum sulfate is dissolved in 175g of water, and then 8.1g of concentrated phosphoric acid (H 3 PO 4 ) fully stirred and mixed evenly, and transferred to the dropping funnel. Heat the reaction kettle to 90°C, start to add phosphoric acid-containing aluminum sulfate solution dropwise, and the dropwise addition is completed in 2 hours, add alkali to adjust the pH value to 2.2, and keep warm for 1 hour to continue the reaction. Filter while hot, and wash the precipitate several times until the conductivity of the washed water is less than 50 μs / cm, then stop washing. Transfer the material to the oven, heat up to 120°C, dry for 60min, the moisture content of the solids is 0.1wt%, th...

Embodiment 2

[0083] The preparation of embodiment 2 crystalline aluminum phosphites

[0084] The preparation process is: add 270g (1mol) aluminum hydrogen phosphite ((H 2 PO 3 ) 3 Al) and the water of 630g, fully stirring and dissolving, obtain aluminum hydrogen phosphite solution. Disperse 78g of aluminum hydroxide in 200g of water in a 500mL beaker and transfer to the dropping funnel. Heat the reaction kettle to 90°C, start dropwise adding the aluminum hydroxide suspension, and complete the dropwise addition in 2 hours, adjust the pH value to 2.6 through the aluminum hydroxide solid, and keep warm for 1 hour to continue the reaction. Filter while hot, and wash the precipitate several times until the conductivity of the washed water is less than 50 μs / cm, then stop washing. Transfer the material to the oven, heat up to 120°C, dry for 60min, the moisture content of the solids is 0.1wt%, then raise the temperature to 180°C at a rate of 2°C / min, keep it for 60min, then raise the temperat...

Embodiment 3

[0096]Adopt the nylon 66 of 52wt%, the glass fiber of 30wt%, the crystalline aluminum phosphite of embodiment 1 of 3.4wt% and 14.6wt% diethylaluminum hypophosphite (LFR8003, Jiangsu Liside New Material Co., Ltd.), according to The general procedure is to prepare flame-retardant glass fiber reinforced nylon 66, and prepare samples to test the flame-retardant performance. The flame-retardant material reaches UL94 V0 (0.8mm).

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Abstract

The invention discloses crystalline aluminum phosphite, a preparation method thereof and application of the crystalline aluminum phosphite as or used for preparing a flame retardant or a flame-retardant synergist. The preparation method comprises the following steps: 1, reacting aluminum hydrogen phosphite and an aluminum-containing compound in water at 80-110 DEG C in the presence or absence of a small amount of strong acid to obtain a precipitate; 2, washing and filtering the precipitate; 3, drying the precipitate at the temperature of 100-130 DEG C to remove water; and 4, continuing to heat and dry the moisture solids at a low-speed gradient temperature rise speed of not more than 5 DEG C / min, and raising the temperature of the materials from normal temperature to not more than 350 DEG C within about 5-10 hours, wherein the temperature rise speed is not more than 5 DEG C / min. Compared with amorphous aluminum phosphite, the crystalline aluminum phosphite has higher thermal decomposition temperature, lower water absorption and weaker acidity, can achieve a synergistic effect with diethyl aluminum hypophosphite, has better flame retardant property, and is used as a halogen-free flame retardant component of a high polymer material.

Description

technical field [0001] The invention relates to the field of material technology, in particular to a crystalline aluminum phosphite and a preparation method and application thereof. Background technique [0002] The mesoscopic state of solid matter includes two aggregate states of crystallization and non-crystallization. Some substances are crystalline substances, and some are non-crystalline substances, which are affected by the chemical composition of the substance; but these aggregation states are also affected by the environmental conditions during preparation, such as temperature, pressure, etc., so the same chemical substance can be expressed as crystallization state, it can also appear as non-crystalline state. The mesoscopic aggregation state of solid substances will affect its physical and chemical properties, such as melting point, solubility, etc. According to different application needs, different mesoscopic aggregation states can be selected. [0003] Aluminum...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/163C09D5/18C08L77/06C08K13/04C08K7/14C08K3/32C08K5/5313C08J5/04C08J5/18D01F1/07D06M11/70D06M101/06D06M101/32
CPCC01B25/163C09D5/18C09D5/185C08J5/043C08K3/32C08J5/18D01F1/07D06M11/70C01P2002/72C08J2377/06C08K13/04C08K7/14C08K5/5313D06M2101/06D06M2101/32D06M2200/30C01P2002/70C01P2004/61C01P2004/62C01P2006/10C08K5/0066C08K3/016D01F1/10C09D7/61C08L77/06C08L67/00C08L73/00C08K3/105C01F7/00C01P2004/60C08K5/53C08K13/02C08K2201/005
Inventor 雷华李金忠
Owner JIANGSU LISIDE NEW MATERIAL
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