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Preparation method of aluminum phenylphosphinate

A technology of aluminum phenylphosphinate and aluminum sulfate, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problem of improving the requirements of feeding equipment and the instability of aluminum chloride hydrolysis , Reduce the utilization rate of aluminum ions and other issues, achieve good hydrolysis stability, suitable for industrial production, and convenient reaction treatment

Active Publication Date: 2013-06-12
NANJING NORMAL UNIVERSITY
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Problems solved by technology

The reaction time of this preparation method is long, and the process is loaded down with trivial details; Nitrogen protection increases cost and has improved the feeding equipment requirement; The pH of the solution of the 2nd step is neutrality to slightly alkaline like this can make Al 3+ Partially converted to Al(OH) 2+ , Al(OH) 2 + , has reduced the utilization rate of aluminum ion; The aluminum chloride used in the 3rd step is unstable because of its hydrolysis, perishable

Method used

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  • Preparation method of aluminum phenylphosphinate
  • Preparation method of aluminum phenylphosphinate

Examples

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Effect test

Embodiment 1

[0033] Add 21.48 g of phenylphosphine dichloride to a 500 ml four-necked flask equipped with a serpentine reflux condenser, an electric stirrer and an acid absorption tower.

[0034] Weigh 15g of aluminum nitrate nonahydrate and dissolve it in 200g of water. Under stirring conditions, slowly drop the aluminum nitrate solution into phenylphosphine dichloride at a temperature range of 0-5°C, adjust the pH to 2-6, heat to 85°C, and react at a constant temperature for 1.5h to obtain a white precipitate, filter and wash , Drying can get white powder product aluminum phenyl phosphinate. The yield was 92.2%.

Embodiment 2

[0036] Add 21.48 g of phenylphosphine dichloride to a 500 ml four-necked flask equipped with a serpentine reflux condenser, an electric stirrer, a constant pressure dropping funnel and an acid absorption tower.

[0037] Weigh 15g of aluminum nitrate nonahydrate and dissolve it in 180g of water. Under stirring conditions, slowly drop the aluminum nitrate solution into phenylphosphine dichloride at a temperature range of 5-10°C, adjust the pH to 2-6, heat to 60°C, and react at constant temperature for 1 hour to obtain a white precipitate, filter, wash, Drying can get white powder product aluminum phenyl phosphinate. The yield was 90.1%.

Embodiment 3

[0039] Add 21.48 g of phenylphosphine dichloride to a 500 ml four-necked flask equipped with a serpentine reflux condenser, an electric stirrer and an acid absorption tower.

[0040] Weigh 15g of aluminum nitrate nonahydrate and dissolve it in 150g of water. Under the condition of stirring, slowly drop the aluminum nitrate solution into the phenylphosphine dichloride in the temperature range of 5-10°C. After dropping, adjust the pH to 2-6, heat to 65°C, and react at constant temperature for 2 hours to obtain a white precipitate, filter , washing, and drying to obtain a white powder product, aluminum phenylphosphinate. The yield was 95.4%.

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Abstract

The invention discloses a preparation method of aluminum phenylphosphinate. The preparation method comprises the following steps: a. preparing 0.1-1mol / L aluminum nitrate or aluminum sulfate solution; b. slowly dropping the aluminum nitrate or aluminum sulfate solution in dichlorophenylphosphine at 0-40 DEG.C; c. after dropping, heating and adjusting the pH value of the solution, reacting for 1-3 hours at 40-100 DEG.C to generate a target product aluminum phenylphosphinate. The method disclosed by the invention is used for preparing aluminum phenylphosphinate by adopting aluminum nitrate or aluminum sulfate solution and dichlorophenylphosphine to directly react under acidic condition in one-step method, the yield of the target product is 87-96%; the obtained aluminum phenylphosphinate is white powder, the color treatment is unnecessary, and the purity is high; the existing process rout is simplified, the reaction time is short, the environment-friendly is realized, the cost is low, and the method is more suitable for the industrial production.

Description

technical field [0001] The invention relates to a preparation method of a flame retardant, in particular to a preparation method of a phenylphosphinate aluminum flame retardant. Background technique [0002] Aluminum phenylphosphinate is white in color, non-toxic, has good thermal stability and hydrolytic stability, is non-volatile, and has good oil resistance. Products made of it will not cause the decomposition of polymers during processing, and will not affect plastics. Molding composition and strong cold and weather resistance. Synergistic use with other flame retardants can complement each other's advantages. It can catalyze the formation of charcoal on the body and enhance the flame retardant performance. It is a highly efficient synergistic flame retardant. [0003] In 2011, Luo Yuan used aluminum phenylphosphinate compounded with melamine pyrophosphate to study the flame retardant modification of glass fiber reinforced polybutylene terephthalate (PBT), [Luo Yuan, Hu...

Claims

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Application Information

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IPC IPC(8): C08K5/5313C07F9/30
Inventor 杨锦飞职慧珍张鹏杨旭峰黄小冬
Owner NANJING NORMAL UNIVERSITY
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