Particle size control method and application of dialkylphosphinate salt

A technology of dialkyl phosphinate and alkyl phosphinate, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problem of large particle size, flame retardant Reduce efficiency, limit applications and other issues, to achieve the effect of simple 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

[0003] Dialkyl phosphinate has been proved to be a highly efficient halogen-free flame retardant and widely used in synthetic materials, but the commonly used dialkyl phosphinate flame retardants are not easy to dissolve due to their large particle size Under the processing temperature, it forms a homogeneous compatible system with the resin, which greatly limits the application of the resin added with this type of flame retardant in thin-walled materials such as film, fiber, and molding.
[0005] However, this method has the following defects: zinc dialkylphosphinate is used to replace aluminum dialkylphosphinate as a flame retardant in resins, because the phosphorus content in zinc dialkylphosphinate is much lower than that of dialkylphosphinate Aluminum phosphonate, causing its flame retardant efficiency to be greatly reduced

Method used

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  • Particle size control method and application of dialkylphosphinate salt
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  • Particle size control method and application of dialkylphosphinate salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Embodiment 1: the preparation of aluminum diethylphosphinate

[0039] Heat 976g (0.8mol) of 10% diethylphosphinic acid solution to 70°C, add 0.01% mass fraction (based on the mass of diethylphosphinic acid solution) of sodium sulfate solution, neutralize with alkali, 45min Add 444g of a mixture of 20% aluminum sulfate (M=666) and water dropwise to form a white solid, cool, filter, wash the precipitate with 2L deionized water, and dry at 180°C for 20h to obtain diethylphosphinic acid Aluminum 101.4g, yield 97.5%, moisture content 0.4%;

[0040] Tap density (g / L): 610; Particle size (μm) distribution: D(10): 10.325; D(50): 26.382; D(90): 53.254;

[0041] IR: 778cm -1 , 1076 cm -1 , 1151cm -1 , 2881 cm -1 , 2959 cm -1 .

Embodiment 2

[0042] Embodiment 2: the preparation of aluminum diethylphosphinate

[0043] Same as Example 1, heat 244g (1mol) of 50% diethylphosphinic acid solution to 100°C, add 0.1% mass fraction (based on the quality of diethylphosphinic acid solution) of sodium sulfate solution, use alkali For neutralization, add 370g of a mixture of 30% by mass aluminum sulfate (M=666) and water dropwise within 40 minutes to form a white solid, cool, filter, wash the precipitate with 2.5L of deionized water, and dry at 180°C for 20 hours to obtain di Aluminum ethyl phosphinate 123.5g, yield 95.0%, moisture content 0.8%;

[0044] Tap density (g / L): 618; Particle size (μm) distribution: D(10): 9.054; D(50): 14.152; D(90): 22.384.

Embodiment 3

[0045] Embodiment 3: the preparation of aluminum diethylphosphinate

[0046] Same as Example 1, heat 305g (0.5mol) 20% diethylphosphinic acid solution to 150°C, add 1% mass fraction (based on the quality of diethylphosphinic acid solution) of sodium sulfate solution, use Alkali neutralization, add dropwise a mixture of 111g of 50% by mass aluminum sulfate (M=666) and water within 0.1h to form a white solid, cool, filter, wash the precipitate with 1L of deionized water, dry at 180°C for 20h, and prepare 61.2 g of aluminum diethylphosphinate was obtained, with a yield of 94.2% and a moisture content of 0.9%;

[0047]Tap density (g / L): 625; particle size (μm) distribution: D(10): 6.586; D(50): 10.581; D(90): 18.469.

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Abstract

The invention discloses a particle size control method of a dialkylphosphinate salt. The particle size control method comprises the following steps: a) adding a strong electrolyte into a water solution of dialkyl phosphinic acid and/or a dialkylphosphinate alkali metal salt to get a strong electrolyte water solution of dialkyl phosphinic acid and/or the dialkylphosphinate alkali metal salt; and b) enabling a mixture of a metal compound and water to react with the strong electrolyte water solution of dialkyl phosphinic acid and/or the dialkylphosphinate alkali metal salt to get the dialkylphosphinate salt as shown in formula (I), wherein R<1> and R<2> are identical or different and represent straight chain or branched chain C1-C6 alkyl; M is Mg, Ca, Al, Sb, Sn, Ge, Ti, Fe, Zr, Zn, Ce, Bi, Sr or Mn; m is 2-4; and the strong electrolyte is a metal salt compound. According to the particle size control method disclosed by the invention, by changing the adding quantity of the strong electrolyte, products with a very small particle size range can be obtained; the method is simple in process and convenient to operate, and production equipment is simplified; and the obtained dialkylphosphinate salt can be applied to production of flame retardants.

Description

technical field [0001] The invention belongs to the field of flame retardant synthesis, and in particular relates to a method for controlling the particle size of a dialkyl phosphinate and an application thereof. Background technique [0002] Polyamide, polyester, unsaturated resin, epoxy resin, polyurethane and other thermoplastic and thermosetting plastics are widely used in construction industry, automobile industry, medical and health care and household appliances. However, these 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 phosphinate has been proved to be a highly efficient halogen-free flame retardant and widely used in synthetic materials, b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30C08K5/5313C08K7/14C08L67/02
Inventor 卢昌利柴生勇李积德孔蕾陈林
Owner ZHUHAI WANTONG CHEM
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