Aluminum diethylphosphinate with high solid-solid phase transition temperature and preparation method thereof

Abstract

The invention provides high solid-solid phase transition temperature aluminum diethylphosphinate and a preparation method thereof. The aluminum diethylphosphinate has a solid-solid phase transition peak at 180 to 200 DEG C. The preparation method comprises: S1, heating a sodium diethylphosphinate solution to a first temperature, adjusting the pH value, adding a potassium permanganate solution intothe solution drop by drop, continuing the reaction and filtering the product to obtain a filtrate, S2, keeping the filtrate at a second temperature, adding an aluminum sulfate solution into the filtrate drop by drop for a reaction and filtering the product to obtain precipitates, and S3, washing and drying the precipitates to obtain the high solid-solid phase transition temperature aluminum diethylphosphinate.

Description

technical field

[0001] The invention relates to an aluminum diethylphosphinate compound with different structures and properties and a preparation method thereof. Background technique

[0002] Aluminum diethylphosphinate is a halogen-free flame retardant with good flame retardant properties. It is widely used in polyester materials, polyamide materials, EVA materials and TPE materials by coordinating with other flame retardants. In the literature, a large number of preparation methods for this material have been reported. For example, Clariant, Guangzhou Jinkai, and Shouguang Weidong have all reported a large amount of synthesis of aluminum diethylphosphinate and its precursor, sodium diethylphosphinate method.

[0003] With people's demand for lightweight, more and more polymer materials are used to replace high-density steel or other alloy materials, and polymers that can be used for a long time at high temperatures have attracted more and more attention. For example, hi...

Examples

preparation example Construction

[0063] In the second embodiment of the present invention, the present invention provides a method for preparing a high solid-solid phase transition temperature compound, comprising:

[0064] S1: heating the sodium diethylphosphinate solution to the first temperature, adjusting the pH, adding potassium permanganate solution dropwise, continuing the reaction and filtering to obtain a filtrate; and

[0065] S2: heat the filtrate described in S1 at a second temperature, add aluminum sulfate solution dropwise to react, and filter to obtain a precipitate; and

[0066] S3: washing and drying the precipitate described in S2 to obtain the compound.

[0067] The raw material sodium diethylphosphinate solution in the present invention is commercially available, and because of the limitation of its preparation process, all contains impurity. According to a preferred embodiment of the present invention, the concentration of the sodium diethylphosphinate solution in the sodium diethylphosp...

Embodiment 1

[0090] Sodium diethylphosphinate solution, configured as 100 liters of 12.5wt% solution, adjust the pH of the solution to 7.0 with 5% sodium hydroxide solution, then heat to 85°C, slowly add 10 g / L potassium permanganate dropwise solution, when just beginning to drop in, the purple color of potassium permanganate disappeared quickly; with the continuous addition of potassium permanganate, the fading became slower and slower, and when the added potassium permanganate solution no longer faded within 30s, Stop the dropwise addition and consume a total of 25.2L of potassium permanganate solution. Filter the mixture to obtain a treated sodium diethylphosphinate solution; in addition, dissolve 10Kg of aluminum sulfate octadecahydrate in 60Kg of water to configure an aluminum sulfate solution, and in the treated sodium diethylphosphinate solution Slowly drop into the aluminum sulfate solution filtered by activated carbon to obtain a large amount of white precipitate, filter, and wash...

Embodiment 2

[0092] Sodium diethylphosphinate solution, configured as 100 liters of 12.5wt% solution, adjusted the pH of the solution to 7.0 with 5% sodium hydroxide solution, then heated to 85°C, and slowly added dropwise 20 g / L of potassium permanganate solution, when just beginning to drop in, the purple color of potassium permanganate disappeared quickly; with the continuous addition of potassium permanganate, the fading became slower and slower, and when the added potassium permanganate solution no longer faded within 30s, Stop the dropwise addition and consume a total of 13L of potassium permanganate solution. The mixture was filtered, and the pH of the solution was adjusted to 3.0-3.8 with 5wt% dilute sulfuric acid to obtain a treated sodium diethylphosphinate solution; in addition, 10Kg of aluminum sulfate octadecadecahydrate was dissolved in 60Kg of water to form an aluminum sulfate solution. Slowly drop the aluminum sulfate solution filtered by activated carbon into the treated s...

technical field

[0001] The invention relates to an aluminum diethylphosphinate compound with different structures and properties and a preparation method thereof. Background technique

[0002] Aluminum diethylphosphinate is a halogen-free flame retardant with good flame retardant properties. It is widely used in polyester materials, polyamide materials, EVA materials and TPE materials by coordinating with other flame retardants. In the literature, a large number of preparation methods for this material have been reported. For example, Clariant, Guangzhou Jinkai, and Shouguang Weidong have all reported a large amount of synthesis of aluminum diethylphosphinate and its precursor, sodium diethylphosphinate method.

[0003] With people's demand for lightweight, more and more polymer materials are used to replace high-density steel or other alloy materials, and polymers that can be used for a long time at high temperatures have attracted more and more attention. For example, hi...

Examples

preparation example Construction

[0063] In the second embodiment of the present invention, the present invention provides a method for preparing a high solid-solid phase transition temperature compound, comprising:

[0064] S1: heating the sodium diethylphosphinate solution to the first temperature, adjusting the pH, adding potassium permanganate solution dropwise, continuing the reaction and filtering to obtain a filtrate; and

[0065] S2: heat the filtrate described in S1 at a second temperature, add aluminum sulfate solution dropwise to react, and filter to obtain a precipitate; and

[0066] S3: washing and drying the precipitate described in S2 to obtain the compound.

[0067] The raw material sodium diethylphosphinate solution in the present invention is commercially available, and because of the limitation of its preparation process, all contains impurity. According to a preferred embodiment of the present invention, the concentration of the sodium diethylphosphinate solution in the sodium diethylphosp...

Embodiment 1

[0090] Sodium diethylphosphinate solution, configured as 100 liters of 12.5wt% solution, adjust the pH of the solution to 7.0 with 5% sodium hydroxide solution, then heat to 85°C, slowly add 10 g / L potassium permanganate dropwise solution, when just beginning to drop in, the purple color of potassium permanganate disappeared quickly; with the continuous addition of potassium permanganate, the fading became slower and slower, and when the added potassium permanganate solution no longer faded within 30s, Stop the dropwise addition and consume a total of 25.2L of potassium permanganate solution. Filter the mixture to obtain a treated sodium diethylphosphinate solution; in addition, dissolve 10Kg of aluminum sulfate octadecahydrate in 60Kg of water to configure an aluminum sulfate solution, and in the treated sodium diethylphosphinate solution Slowly drop into the aluminum sulfate solution filtered by activated carbon to obtain a large amount of white precipitate, filter, and wash...

Embodiment 2

[0092] Sodium diethylphosphinate solution, configured as 100 liters of 12.5wt% solution, adjusted the pH of the solution to 7.0 with 5% sodium hydroxide solution, then heated to 85°C, and slowly added dropwise 20 g / L of potassium permanganate solution, when just beginning to drop in, the purple color of potassium permanganate disappeared quickly; with the continuous addition of potassium permanganate, the fading became slower and slower, and when the added potassium permanganate solution no longer faded within 30s, Stop the dropwise addition and consume a total of 13L of potassium permanganate solution. The mixture was filtered, and the pH of the solution was adjusted to 3.0-3.8 with 5wt% dilute sulfuric acid to obtain a treated sodium diethylphosphinate solution; in addition, 10Kg of aluminum sulfate octadecadecahydrate was dissolved in 60Kg of water to form an aluminum sulfate solution. Slowly drop the aluminum sulfate solution filtered by activated carbon into the treated s...

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