Preparation method of dialkylphosphinate metal salt

A technology of dialkylphosphinic acid and dialkylphosphinic acid, which is applied in the field of preparation of dialkylphosphinic acid metal salts, can solve the problems of difficult resin mixing, low tap density, poor fluidity, etc., and achieve simplification The effect of production equipment, small particle size and convenient operation

Inactive Publication Date: 2013-06-26
ZHUHAI WANTONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to overcome the problems of the existing dialkylphosphinic acid metal salt flame retardants such as low tap density, poor fluidity, easy to raise dust, and difficult to mix with resin, the purpose of the present invention is to provide a kind of flame retardant with small particle size and high density. The preparation method of dialkyl phosphinic acid metal salt with good fluidity and easy uniform distribution in resin

Method used

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  • Preparation method of dialkylphosphinate metal salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] To prepare aluminum diethylphosphinate, heat 1440g (3mol) 30% sodium diethylphosphinate solution to 95°C, add 0.01% mass fraction (based on the mass of sodium diethylphosphinate solution) Silane coupling agent KH560, add 333g of aluminum sulfate (M=666) solid within 25min to form a white solid, cool, filter, wash the precipitate with 6L of deionized water, and dry at 200°C for 16h. 383.4 g of aluminum diethylphosphinate was obtained, with a yield of 98.3% and a moisture content of 0.2%.

[0046] Tap density (g / L): 562; Particle size (μm) distribution: D(10): 18.672; D(50): 56.348; D(90): 77.549

[0047] IR: 779cm -1 , 1076 cm -1 , 1151 cm -1 , 2879 cm -1 , 2959 cm -1

Embodiment 2

[0049] Prepare aluminum diethylphosphinate as in Example 1, heat 822.9g (4mol) of 70% sodium diethylphosphinate solution to 150°C, in 4440g of 10% aluminum sulfate by mass (M=666) Add 0.5% mass fraction of silane coupling agent KH560 (based on the mass of aluminum sulfate solution) to the mixture of water and water, and add the aluminum sulfate solution to the sodium diethylphosphinate solution dropwise within 10 hours to form a white solid , cooled, filtered, washed the precipitate with 8L deionized water, and dried at 200°C for 16h. 507.5 g of aluminum diethylphosphinate was obtained, with a yield of 97.6% and a moisture content of 0.3%.

[0050] Tap density (g / L): 571; Particle size (μm) distribution: D(10): 12.248; D(50): 41.471; D(90): 63.825

Embodiment 3

[0052] Prepare aluminum diethylphosphinate with Example 1, heat 1728g (1.2mol) 10% sodium diethylphosphinate solution to 100°C, add 0.1% mass fraction (based on the amount of sodium diethylphosphinate solution The mass fraction of the silane coupling agent KH560, 0.05% mass fraction of the silane coupling agent KH560 (based on the mass percentage of aluminum sulfate solution of Benchmark), add the aluminum sulfate solution dropwise to the sodium diethylphosphinate solution within 1 hour to form a white solid, cool, filter, wash the precipitate with 2L of deionized water, and dry at 200°C for 16 hours. 151.0 g of aluminum diethylphosphinate was obtained, with a yield of 96.8% and a moisture content of 0.5%.

[0053] Tap density (g / L): 610; Particle size (μm) distribution: 13.219; D(50): 45.387; D(90): 70.516

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Abstract

The invention discloses a preparation method of a dialkylphosphinate metal salt. The preparation method comprises the following steps: a) adding a coupling agent into a water solution of dialkyl phosphinic acid and/or a dialkylphosphinate alkali metal salt to get the water solution of dialkyl phosphinic acid and/or the dialkylphosphinate alkali metal salt containing the coupling agent; and b) adding the coupling agent or not adding the coupling agent into a mixture of a metal compound and water, and further reacting with the water solution of dialkyl phosphinic acid and/or the dialkylphosphinate alkali metal salt containing the coupling agent to generate the dialkylphosphinate metal salt. The dialkylphosphinate metal salt obtained by the preparation method disclosed by the invention has small particle size and good flowability; and furthermore, when the particle size is less than 90 mu m, in particular to 40 mu m, the tap density can still above 600g/L, and the problems that such flame retardants are easy to raise dust during the feeding process and less prone to uniformly mixing with resin can be well solved. The preparation method disclosed by the invention has the advantages of simple process and convenience in operation, and the coupling agent is low in price and easy to obtain; and simultaneously, production equipment is simplified and production cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of flame retardant synthesis, and in particular relates to a method for preparing dialkylphosphinic acid metal salts with small particle size and high density. Background technique [0002] Polymer materials (plastics, rubber, synthetic fibers, etc.) are widely used in construction, automobiles, medical and health care, and household appliances because of their light weight, low price, and corrosion resistance. However, polymer materials are usually flammable or combustible, and the requirements for their flame retardancy are getting higher and higher in practical applications. In order to ensure the safety of synthetic materials and meet the requirements of environmental protection, the most effective method is to add halogen-free flame retardants to synthetic materials. [0003] Dialkyl phosphinates have been proven to be highly efficient halogen-free flame retardants and are widely used in synthetic mate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30C08K5/5313C08L67/02
Inventor 卢昌利柴生勇李积德孔蕾陈林
Owner ZHUHAI WANTONG CHEM
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