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Method for preparing phosphinic acid modified aluminum hydroxide flame retardant agents

A kind of aluminum hydroxide flame retardant, aluminum hydroxide technology, applied in dyeing low molecular organic compound treatment, fibrous filler, etc., can solve the problems of damaged material performance, poor compatibility, etc., to block the source of combustion and isolate oxygen , the effect of excellent heat resistance

Inactive Publication Date: 2012-01-25
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, when aluminum hydroxide is directly used as a flame retardant for the flame retardant modification of synthetic resins, there are two shortcomings: (1) The filling amount of aluminum hydroxide must be more than 50%, so that the composite material can show better performance. (2) Due to the poor compatibility between the larger inorganic particles and the resin, the performance of the material, especially the mechanical properties, will be seriously damaged when the filling amount is large.

Method used

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  • Method for preparing phosphinic acid modified aluminum hydroxide flame retardant agents
  • Method for preparing phosphinic acid modified aluminum hydroxide flame retardant agents
  • Method for preparing phosphinic acid modified aluminum hydroxide flame retardant agents

Examples

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Embodiment 1

[0031] What this embodiment prepares is organic phosphinic acid modified aluminum hydroxide flame retardant, specific steps and conditions are:

[0032] Diallylphosphinic acid modified aluminum hydroxide 2.8g (19.2mmol) diallylphosphinic acid, and 30ml acetic acid, deoxygenated with nitrogen, and added 1.0g aluminum hydroxide under stirring. After reacting at room temperature for 36 hours, the white precipitate was collected, filtered, washed with deionized water, ethanol, and acetone, and then vacuum-dried at 50° C. for 12 hours to obtain a fluffy white powder. Initial decomposition temperature: 278.0°C, weight loss: 19.5%. Secondary decomposition temperature: 488.6°C, weight loss: 26.8%.

Embodiment 2

[0034] What this embodiment prepares is organic phosphinic acid modified aluminum hydroxide flame retardant, specific steps and conditions are:

[0035] Bis(3-methoxy-3-oxopropyl)phosphinic acid modified aluminum hydroxide method is the same as case 5, finally get a white precipitate, filter, wash with deionized water, ethanol, acetone respectively, and then incubate at 50°C Dry under vacuum for 12 hours. The initial decomposition temperature is: 280.7°C, and the weight loss is: 16.3%. Secondary decomposition temperature: 382.0°C, weight loss: 30.6%.

Embodiment 3

[0037] What this embodiment prepares is organic phosphinic acid modified aluminum hydroxide flame retardant, specific steps and conditions are:

[0038] The method for modifying aluminum hydroxide with dibenzylphosphinic acid is the same as that of Case 5. Finally, a white precipitate is obtained, which is filtered, washed with deionized water, ethanol, and acetone, and then vacuum-dried at 50°C for 12 hours. The initial decomposition temperature is: 268.2°C, and the weight loss is: 4.47%. Secondary decomposition temperature: 495.9°C, weight loss: 65.5%.

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Abstract

The invention discloses a method for preparing phosphinic acid modified aluminum hydroxide flame retardant agents, which is characterized by comprising the following steps that: the aluminum hydroxide is taken, the organic solvent glacial acetic acid is taken according to the proportion being 10 to 15 times of the mass of the aluminum hydroxide, and the organic phosphinic acid is taken according to the mol ratio of the aluminum hydroxide to the organic phosphinic acid of 1 / 1.0 to 2.0; the aluminum hydroxide is dispersed in the organic solvent glacial acetic acid, the organic phosphinic acid is added into the aluminum hydroxide dispersing liquid during stirring, the reaction is carried out for 24 to 36h at the room temperature to 80 DEG C after the nitrogen gas is introduced for 10 to 30 minutes, and reacted materials are obtained; and the reacted materials are filtered while being hot, solid materials are washed and dried, and the phosphinic acid modified aluminum hydroxide flame retardant agents are prepared. When the method is adopted, the prepared phosphinic acid modified aluminum hydroxide flame retardant agents have better heat stability and hydrophobicity and are used in epoxy resin composite materials, the mechanical performance and the like of the composite materials are obviously improved, and the flame retardant performance is good.

Description

technical field [0001] The invention belongs to a preparation method of organic polymer compound batching, and relates to a preparation method of a phosphinic acid modified aluminum hydroxide flame retardant. The prepared phosphinic acid-modified aluminum hydroxide flame retardant is suitable for flame-retardant modification of epoxy resin, especially suitable for flame-retardant modification of bisphenol A glycidyl ether type epoxy resin. Background technique [0002] Epoxy resin, due to its excellent properties such as low density, biocompatibility and biodegradability, good transparency, resistance to heat and humidity, and easy processing, has been rapidly developed in various fields. However, there is a big disadvantage of epoxy resin, that is, epoxy resin is easy to burn during application, especially when it is used in construction industry, electronic circuit and aerospace. The flame retardant modification of epoxy resin can effectively improve its shortcomings such...

Claims

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Application Information

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IPC IPC(8): C09C1/40C09C3/08C08K9/04C08K3/22C08L63/00C08L63/02
Inventor 杨军校马佳俊曹克黄亚文
Owner SOUTHWEAT UNIV OF SCI & TECH
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