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Preparation method and application of large-particle-size spherical dialkylphosphinate

A technology of alkyl phosphinate and dialkyl phosphinic acid, which is applied in the field of preparation of large particle size spherical dialkyl phosphinate, to achieve the effect of improving equipment production capacity, simple filtration process, and regular shape

Active Publication Date: 2017-05-10
ZHEJIANG TRANSFAR WHYYON CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by the present invention is to overcome the defects in the preparation and use of the above-mentioned existing dialkyl phosphinates, and provide a method for preparing spherical dialkyl phosphinates with large particle size, so that dialkyl phosphinates The preparation process of the base phosphinate is simple to operate, the reaction conditions are mild, the reaction time is short, the energy consumption is low, the corrosion is small, the pollution is small, the product is pure, and the yield is high, so it is more suitable for practical use and has industrial utilization value

Method used

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  • Preparation method and application of large-particle-size spherical dialkylphosphinate
  • Preparation method and application of large-particle-size spherical dialkylphosphinate
  • Preparation method and application of large-particle-size spherical dialkylphosphinate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Add 150 g of sodium diethylphosphinate and 600 mL of water into a 2000 mL four-necked flask equipped with a reflux condenser, an electric stirrer and a thermometer. With stirring, the solution was heated to 80°C.

[0042] 1.2 g of melamine polyphosphate was added to 50 g of 50% ethanol aqueous solution, and then 0.6 g of polyvinylpyrrolidone was added. With high speed stirring, the solution was heated to 50°C. After uniform dispersion, it was added to a four-necked flask to form a mixed solution.

[0043] The mixed solution was heated to 120°C under stirring and under pressure. Within 2.5 hours, 800 mL of a solution containing 115 g of aluminum sulfate octadecahydrate was added dropwise to the above mixed solution, and the mixture was reacted under pressure for 2 hours to obtain a white precipitate. Cool to room temperature, filter, wash, and dry to obtain a white powder product. The yield was 90.5%.

[0044] The product particle size (μm) distribution is: D(10): 2...

Embodiment 2

[0047] Add 150 g of sodium diethylphosphinate and 500 mL of water into a 2000 mL four-necked flask equipped with a reflux condenser, an electric stirrer and a thermometer. With stirring, the solution was heated to 90°C.

[0048] 1.0 g of melamine cyanurate was added to 50 g of 50% ethanol aqueous solution, and then 0.6 g of sodium dodecylbenzenesulfonate was added. With high speed stirring, the solution was heated to 50°C. After uniform dispersion, it was added to a four-necked flask to form a mixed solution.

[0049] Within 2.5 hours, 700 mL of a solution containing 115 g of aluminum sulfate octadecahydrate was added dropwise to the above mixed solution, and the mixture was incubated for 2 hours to obtain a white precipitate. Cool to room temperature, filter, wash, and dry to obtain a white powder product. The yield was 91.9%.

[0050] Product particle size (μm) distribution is: D(10):20; D(25):31; D(50):45; D(97):101;

[0051] TGA: T1% = 380°C.

Embodiment 3

[0053] Add 150 g of sodium diethylphosphinate and 900 mL of water into a 2000 mL four-necked flask equipped with a reflux condenser, an electric stirrer and a thermometer. With stirring, the solution was heated to 80°C.

[0054] 0.8 g of melamine was added to 50 g of 50% methanol aqueous solution, and then 0.8 g of potassium dodecyl phosphate was added. With high speed stirring, the solution was heated to 50°C. After uniform dispersion, it was added to a four-necked flask to form a mixed solution.

[0055] Within 2.0 h, 900 mL of a solution containing 115 g of aluminum sulfate octadecahydrate was added dropwise to the above mixed solution, and kept for 2 h to obtain a white precipitate. Cool to room temperature, filter, wash, and dry to obtain a white powder product. The yield was 89.5%.

[0056] Product particle size (μm) distribution is: D(10): 15; D(25): 28; D(50): 35; D(97): 99;

[0057] TGA: T1% = 386°C.

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Abstract

The invention discloses a preparation method and application of large-particle-size spherical dialkylphosphinate. Preparation methods and application of present dialkylphosphinate have many defects. The preparation method of the invention comprises the steps of 1) preparing dialkylphosphinic acid or / and dialkylphosphinate into a solution; 2) adding a compound, dissolved in an alcohol or / or aqueous solution and containing nitrogen or both nitrogen and phosphorus, as precipitation seed crystal into the solution of dialkylphosphinic acid or / and dialkylphosphinate, and adding suitable surfactant to provide improved dispersion to obtain mixed solution; 3) dropwise adding soluble metal salt solution into the above mixed solution, cooling after reacting, filtering, washing, and drying to obtain the large-particle-size spherical dialkylphosphinate. The large-particle-size spherical dialkylphosphinate of the invention can be added to a polymer material as a halogen-free flame retardant in order to improve polymer mobility, and the mixing effect is significant.

Description

technical field [0001] The invention belongs to the technical field of flame retardant preparation, in particular to a preparation method and application of a spherical dialkyl phosphinate with large particle size. Background technique [0002] The phosphorus content in dialkylphosphinate (structural formula as shown below) is relatively high, and the main chemical bonds are P-C, P=O and P-O. It has good thermal stability, low water solubility, and has both condensed phase flame retardancy and Vapor-phase flame retardant has been used as a substitute for brominated flame retardants in the flame retardant of polymer materials, and the flame retardant effect is good. Dialkyl phosphinate is used in engineering plastics such as polyamide and polyester, the heat release rate and the heat generated during combustion are drastically reduced, the flame retardancy is good, and the CTI value is high. [0003] [0004] Dialkyl phosphinate can be prepared by various methods, for exa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30C08L77/06C08L67/02C08K7/14C08K7/16C08K5/3492
CPCC07F9/301C07F9/304C08K5/34928C08K7/14C08K7/16C08L2201/02C08L77/06C08L67/02
Inventor 陈俊童敏伟屈亚平张小英葛琴琴汪义钧乔涛
Owner ZHEJIANG TRANSFAR WHYYON CHEM
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