Method for producing aluminium hypophosphite by adopting reaction extrusion process

A technology of reactive extrusion and aluminum hypophosphite, which is applied in the direction of hypophosphorous acid and phosphorus oxyacid, can solve the problems of lower decomposition temperature of aluminum hypophosphite and large particle size of aluminum hypophosphite, so as to reduce energy consumption and production cost Low, high yield effect

Inactive Publication Date: 2014-06-25
广东宇星阻燃新材股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Because the particle size of the aluminum hypophosphite particles obtained by the above method is relatively large, the crystallization of the by-product sodium sulfate is easily mixed in the process of aluminum hypophosphite crystallization, resulting in a reduction in the decomposition temperature of the finished product aluminum hypophosphite

Method used

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  • Method for producing aluminium hypophosphite by adopting reaction extrusion process
  • Method for producing aluminium hypophosphite by adopting reaction extrusion process
  • Method for producing aluminium hypophosphite by adopting reaction extrusion process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A method for producing aluminum hypophosphite using a reactive extrusion process, including the following steps:

[0035] (1) Mix 5280g of sodium hypophosphite and 3420g of aluminum sulfate uniformly, then add the mixture into a twin-screw extruder set at 50°C for reactive extrusion; after reactive extrusion, a white mud-like product is obtained;

[0036] (2) The product of step (1) is sealed and stored in an environment of 50° C., and matured for 24 hours; then the product is washed, filtered and dried to obtain white powdery aluminum hypophosphite. After testing, the yield of the product obtained in this example was 98%. The particle size analysis of the obtained aluminum hypophosphite is shown in Table 1, and the infrared detection spectrum is shown in figure 1 , See the thermal weight loss chart figure 2 And table 2.

Embodiment 2

[0047] A method for producing aluminum hypophosphite using a reactive extrusion process, including the following steps:

[0048] (1) Mix 2490g of ammonium hypophosphite and 2130g of aluminum nitrate uniformly, then add the mixture into a twin-screw extruder set at 70°C for reactive extrusion; after reactive extrusion, a white mud-like product is obtained;

[0049] (2) The product of step (1) is sealed and stored in an environment of 80° C., and matured for 4 hours; then the product is washed, filtered and dried to obtain white powdery aluminum hypophosphite. After testing, the yield of the product obtained in this example was 97%. The particle size analysis of the obtained aluminum hypophosphite is shown in Table 3, and the infrared detection spectrum is shown in image 3 , See the thermal weight loss chart Figure 4 And Table 4.

[0050] Table 3 Particle size analysis of aluminum hypophosphite prepared in Example 2 and Comparative Example 1

[0051]

Median diameter

Volume ave...

Embodiment 3

[0056] A method for producing aluminum hypophosphite using a reactive extrusion process, including the following steps:

[0057] (1) Mix 3122g potassium hypophosphite and 1333g aluminum chloride uniformly, then add the mixture into a twin-screw extruder set at 60°C for reactive extrusion; after reactive extrusion, a white mud-like product is obtained;

[0058] (2) The product of step (1) is sealed and stored in an environment of 60° C., and matured for 12 hours; then the product is washed, filtered and dried to obtain white powdery aluminum hypophosphite. After testing, the yield of the product obtained in this example was 98%. The particle size analysis of the obtained aluminum hypophosphite is shown in Table 5, and the infrared detection spectrum is shown in Figure 5 , See the thermal weight loss chart Image 6 And table 6.

[0059] Table 5 Particle size analysis of aluminum hypophosphite prepared in Example 3 and Comparative Example 1

[0060]

Median diameter

Volume averag...

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Abstract

The invention discloses a method for producing aluminium hypophosphite by adopting a reaction extrusion process. The method comprises the following steps: (1) uniformly mixing hypophosphite and aluminium salt or hypophosphorous acid and aluminium hydroxide or hypophosphorous acid and aluminium oxide, and carrying out reaction extrusion on a double screw extruder; (2) aging a product obtained from the step (1) at 20-80 DEG C for 4-48 hours, and then washing, filtering and drying the product to obtain the aluminium hypophosphite. According to the method, a reactant can be fast reacted due to high torque and high rotation speed of the double screw extruder, so that the reaction time can be shortened, and the energy consumption can be reduced; an aluminium hypophosphite granule with the grain diameter less than 10 micrometers can be obtained.

Description

Technical field [0001] The invention belongs to the technical field of aluminum hypophosphite preparation, and specifically relates to a method for producing aluminum hypophosphite by a reactive extrusion process. Background technique [0002] Aluminum hypophosphite is a new type of inorganic phosphorus flame retardant with the chemical formula of Al(H2PO2)3. It has the advantages of being slightly soluble in water, non-volatile, high phosphorus content, and good thermal stability. High flammability, strong thermal stability, and excellent mechanical properties and weather resistance. At present, the production of aluminum hypophosphite mainly uses sodium hypophosphite and aluminum sulfate as raw materials, which are heated and reacted in the water phase to obtain aluminum hypophosphite particles, which are dried and pulverized to obtain dry powder. [0003] Due to the large particle size of the aluminum hypophosphite particles obtained by the above method, the by-product sodium s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/165
Inventor 罗宏波马访中甄利军罗章志刘敏顾湘
Owner 广东宇星阻燃新材股份有限公司
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