Modified phosphorus-nitrogen type flame retardant and preparation method thereof

Abstract

The invention provides a modified phosphorus-nitrogen type flame retardant and a preparation method thereof. The preparation method comprises the following steps: adding pentaerythritol into a three-neck flask, putting the flask into an ice-water bath, stirring for 30 minutes at the rotating speed of 100 to 120 r / min, dropwise adding phosphorus oxychloride while stirring, controlling the dropwiseadding time to be 15 minutes, absorbing tail gas by using a sodium hydroxide aqueous solution with the mass fraction of 20% in the dropwise adding process, after dropwise adding is finished, stirringfor 30 minutes at a constant speed, then heating to 60 to 70 DEG C, and stirring for 2 hours at a constant speed at the temperature. In the step S3, melamine and cyanuric acid are mixed and subjectedto hydrogen bond compounding, then a mixed solution A prepared from a second product is added, and the second product is added, so that the formation of a melamine cyanurate large-plane network structure can be interfered and inhibited, the particle size is refined. and the prepared modified phosphorus-nitrogen type flame retardant has good dispersity.

Description

technical field

[0001] The invention belongs to the technical field of flame retardant preparation, in particular to a modified phosphorus-nitrogen type flame retardant and a preparation method thereof. Background technique

[0002] Flame retardants can be divided into additive type and reactive type according to the processing method. The additive type is cheap and easy to operate, occupying most of the flame retardant market share, but the additive type flame retardant has poor compatibility with polymers, easy to bloom, and easy to migrate, which makes the flame retardant performance of the material change over time. In addition, the additive flame retardant has a certain influence on the processing and physical and mechanical properties of polymer materials. Although the processing of reactive flame retardants is relatively complicated and the cost is slightly higher, it will not cause compatibility problems, and at the same time, it will have very little impact on the ...

Examples

Embodiment 1

[0028] A modified phosphorus nitrogen type flame retardant, made by the following method:

[0029] Step S1. Add pentaerythritol into a three-necked flask, place it in an ice-water bath, stir at a speed of 100r / min for 30min, add phosphorus oxychloride dropwise while stirring, control the dropping time to 15min, and use a mass fraction of 20% during the dropping process. % sodium hydroxide aqueous solution to absorb the tail gas, stir at a constant speed for 30 minutes after the dropwise addition, then raise the temperature to 60°C, stir at a constant speed at this temperature for 2 hours, heat up to 100°C, reflux until no hydrogen chloride is produced, cool and filter with suction after the reaction , the filter cake was washed three times with chloroform and absolute ethanol, and then transferred to a vacuum drying oven with a vacuum degree of -0.10 MPa, and dried at 50°C for 10 hours to obtain the first product. In step S1, pentaerythritol and three The weight ratio of phosp...

Embodiment 2

[0036] A modified phosphorus nitrogen type flame retardant, made by the following method:

[0037] Step S1. Add pentaerythritol into a three-necked flask, place it in an ice-water bath, stir at a speed of 100r / min for 30min, add phosphorus oxychloride dropwise while stirring, control the dropping time to 15min, and use a mass fraction of 20% during the dropping process. % sodium hydroxide aqueous solution to absorb the tail gas, stir at a constant speed for 30 minutes after the dropwise addition, then raise the temperature to 60°C, stir at a constant speed at this temperature for 2 hours, heat up to 100°C, reflux until no hydrogen chloride is produced, cool and filter with suction after the reaction , the filter cake was washed three times with chloroform and absolute ethanol, and then transferred to a vacuum drying oven with a vacuum degree of -0.10 MPa, and dried at 50°C for 10 hours to obtain the first product. In step S1, pentaerythritol and three The weight ratio of phosp...

Embodiment 3

[0044] A modified phosphorus nitrogen type flame retardant, made by the following method:

[0045] Step S1. Add pentaerythritol into a three-necked flask, place it in an ice-water bath, stir at a speed of 100r / min for 30min, add phosphorus oxychloride dropwise while stirring, control the dropping time to 15min, and use a mass fraction of 20% during the dropping process. % sodium hydroxide aqueous solution to absorb the tail gas, stir at a constant speed for 30 minutes after the dropwise addition, then raise the temperature to 60°C, stir at a constant speed at this temperature for 2 hours, heat up to 100°C, reflux until no hydrogen chloride is produced, cool and filter with suction after the reaction , the filter cake was washed three times with chloroform and absolute ethanol, and then transferred to a vacuum drying oven with a vacuum degree of -0.10 MPa, and dried at 50°C for 10 hours to obtain the first product. In step S1, pentaerythritol and three The weight ratio of phosp...

technical field

[0001] The invention belongs to the technical field of flame retardant preparation, in particular to a modified phosphorus-nitrogen type flame retardant and a preparation method thereof. Background technique

[0002] Flame retardants can be divided into additive type and reactive type according to the processing method. The additive type is cheap and easy to operate, occupying most of the flame retardant market share, but the additive type flame retardant has poor compatibility with polymers, easy to bloom, and easy to migrate, which makes the flame retardant performance of the material change over time. In addition, the additive flame retardant has a certain influence on the processing and physical and mechanical properties of polymer materials. Although the processing of reactive flame retardants is relatively complicated and the cost is slightly higher, it will not cause compatibility problems, and at the same time, it will have very little impact on the ...

Examples

Embodiment 1

[0028] A modified phosphorus nitrogen type flame retardant, made by the following method:

[0029] Step S1. Add pentaerythritol into a three-necked flask, place it in an ice-water bath, stir at a speed of 100r / min for 30min, add phosphorus oxychloride dropwise while stirring, control the dropping time to 15min, and use a mass fraction of 20% during the dropping process. % sodium hydroxide aqueous solution to absorb the tail gas, stir at a constant speed for 30 minutes after the dropwise addition, then raise the temperature to 60°C, stir at a constant speed at this temperature for 2 hours, heat up to 100°C, reflux until no hydrogen chloride is produced, cool and filter with suction after the reaction , the filter cake was washed three times with chloroform and absolute ethanol, and then transferred to a vacuum drying oven with a vacuum degree of -0.10 MPa, and dried at 50°C for 10 hours to obtain the first product. In step S1, pentaerythritol and three The weight ratio of phosp...

Embodiment 2

[0036] A modified phosphorus nitrogen type flame retardant, made by the following method:

[0037] Step S1. Add pentaerythritol into a three-necked flask, place it in an ice-water bath, stir at a speed of 100r / min for 30min, add phosphorus oxychloride dropwise while stirring, control the dropping time to 15min, and use a mass fraction of 20% during the dropping process. % sodium hydroxide aqueous solution to absorb the tail gas, stir at a constant speed for 30 minutes after the dropwise addition, then raise the temperature to 60°C, stir at a constant speed at this temperature for 2 hours, heat up to 100°C, reflux until no hydrogen chloride is produced, cool and filter with suction after the reaction , the filter cake was washed three times with chloroform and absolute ethanol, and then transferred to a vacuum drying oven with a vacuum degree of -0.10 MPa, and dried at 50°C for 10 hours to obtain the first product. In step S1, pentaerythritol and three The weight ratio of phosp...

Embodiment 3

[0044] A modified phosphorus nitrogen type flame retardant, made by the following method:

[0045] Step S1. Add pentaerythritol into a three-necked flask, place it in an ice-water bath, stir at a speed of 100r / min for 30min, add phosphorus oxychloride dropwise while stirring, control the dropping time to 15min, and use a mass fraction of 20% during the dropping process. % sodium hydroxide aqueous solution to absorb the tail gas, stir at a constant speed for 30 minutes after the dropwise addition, then raise the temperature to 60°C, stir at a constant speed at this temperature for 2 hours, heat up to 100°C, reflux until no hydrogen chloride is produced, cool and filter with suction after the reaction , the filter cake was washed three times with chloroform and absolute ethanol, and then transferred to a vacuum drying oven with a vacuum degree of -0.10 MPa, and dried at 50°C for 10 hours to obtain the first product. In step S1, pentaerythritol and three The weight ratio of phosp...

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