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Hydroxy aluminium oxalate, and its preparing method and hydroxy aluminium oxalate as fire retardant

A technology of hydroxyaluminum oxalate and hydroxyoxalic acid, which is applied in the preparation of carboxylate, organic chemistry, etc., can solve the problems of complex structure of rotating bed equipment, high viscosity of hydrated alumina, inconvenient maintenance and disassembly, etc., and achieve simple structure and low weight loss temperature High and stable product quality

Inactive Publication Date: 2006-03-29
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The structure of the rotating bed equipment used in this method is relatively complex, there are many auxiliary equipment, it is inconvenient to maintain and disassemble, and due to the high viscosity of hydrated alumina, it is easy to cause blockage of the channel.
In addition, due to the circulating flow of slurry, the power consumption is large

Method used

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  • Hydroxy aluminium oxalate, and its preparing method and hydroxy aluminium oxalate as fire retardant
  • Hydroxy aluminium oxalate, and its preparing method and hydroxy aluminium oxalate as fire retardant
  • Hydroxy aluminium oxalate, and its preparing method and hydroxy aluminium oxalate as fire retardant

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Add 45 grams of industrial sodium hydroxide to 100 ml of tap water, heat, add 65 grams of industrial aluminum hydroxide after the solution boils, boil for 30 minutes, then add tap water to 800 ml, filter, and remove impurities to obtain partial aluminum Sodium acid solution, its concentration is about 1.0mol / L. Put this sodium metaaluminate solution in a stirred reaction kettle, at 20°C, let in the carbon dioxide gas from the decompressed steel cylinder, and start the agitator at the same time, when the pH value of the solution becomes 10.5, the carbonization and decomposition will end reaction. The resulting slurry is filtered and washed to obtain an aluminum hydroxide filter cake. Then stir the filter cake with deionized water, add solid oxalic acid, make a suspension according to the molar ratio of aluminum hydroxide and oxalic acid 1:0.7, put it in an autoclave for modification treatment, heat it to a temperature of 160°C, and 45 minutes at constant temperature. ...

Embodiment 2

[0042] Except that following operating conditions change, all the other are the same as embodiment 1. 108 grams of sodium hydroxide are added to 150 milliliters of tap water, and the aluminum hydroxide of 158 grams is added after being heated to solution boiling. Continue heating, boil for 30 minutes, and obtain a sodium metaaluminate solution with a concentration of about 2.5mol / L after filtering. It is carbonized and decomposed at 60°C, and the pH value of the end point of carbonization is 11.5. During the modification treatment, the constant temperature was 180° C., the time was 30 minutes, and the molar ratio of oxalic acid to aluminum hydroxide was 1. The slurry obtained after modification is directly filtered, washed, and the filter cake is dried without adding a crystal form control agent to obtain a hydroxyaluminum oxalate product.

Embodiment 3

[0044] Except that following operating conditions change, all the other are the same as embodiment 1. During the modification process, the temperature was maintained at 170° C. for 60 minutes. The prepared modified slurry is directly filtered, washed and the filter cake is dried without adding a crystal form control agent to obtain a chain-like spherical hydroxyaluminum oxalate product. Its TEM picture is shown in Figure 5 , the extrapolated initial weight loss temperature is 356°C, the peak temperature is 399°C, the weight loss rate before 500°C is 50.73%, and its bulk density is 0.51g / cm 3 , the compact density is 0.87g / cm 3 .

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Abstract

The present invention is the aluminum hydroxyoxalate and its preparation process. Aluminum hydroxyoxalate is used as fire retardant, and has molecular expression of Al2(C2O4)(OH)4, and X-ray diffraction spectrum with strong diffraction peaks at D values one 6.5149, 4.7263 and 4.2957 angstrom. Aluminum hydroxyoxalate is prepared through carbonization and decomposition and modification treatment, and through further crystal form controlling treatment, aluminum hydroxyoxalate with high dispersivity and complete crystal form may be obtained. Aluminum hydroxyoxalate has minimum one-dimensional size controlled in 40 nanometers to several microns, extrapolation onset weight-loss temperature higher than 340 deg.c, and weight-loss rate before 500 deg.c up to 51 %. As one kind of green fire retardant, aluminum hydroxyoxalate may be used in thermoplastic plastic and other polymer material with processing temperature over 210 deg.c.

Description

field of invention [0001] The invention relates to hydroxyaluminum oxalate and a preparation method thereof. The hydroxyaluminum oxalate is prepared by carbonization, decomposition and modification of sodium metaaluminate solution and carbon dioxide. It is a flame retardant and can be used for flame retardant of polymer materials. Background technique [0002] Since engineering plastics are widely used in human's daily life, its flame retardant performance has been paid more and more attention. At present, flame-retardant thermoplastic engineering plastics usually use additive flame retardants, and the most commonly used ones are organic halogen flame retardants. As we all know, halogen flame retardants have a large amount of smoke during combustion, and release toxic and corrosive hydrogen halide gas. Inorganic flame retardants have the characteristics of halogen-free, non-toxic, low-smoke, etc., but they have the disadvantages of large amount of addition and poor affinity...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C55/07C07C51/41C08K5/098C09K21/00
Inventor 郭奋陈建峰张纪尧马淑花
Owner BEIJING UNIV OF CHEM TECH
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