Symtriazine-type flame retardant, preparation method and application of symtriazine-type flame retardant

Abstract

The invention discloses a smtriazine-type flame retardant, a preparation method and application of the smtriazine-type flame retardant. The structure of the smtriazine-type flame retardant is shown as a formula I, the method is easy in preparation and easy to implement, and the prepared smtriazine-type flame retardant is high in heat stability and excellent in physical and mechanical properties. The method comprises the following steps: mixing and dissolving cyanuric chloride and acetone, reducing the temperature, continuously dripping an aqueous solution of potassium carbonate to regulate the pH to be 5-7, reacting at the temperature of 15-45 DEG C for 15-60 minutes after dripping, and performing aftertreatment to obtain the smtriazine-type flame retardant. In the used method for preparing the smtriazine-type flame retardant, the raw materials are readily available; the obtained smtriazine-type flame retardant is white in color, excellent in heat stability and physical and mechanical properties and high in yield; a fabric finished by the flame retardant is small in combustion smoke amount, high in char yield and environmentally friendly and can obtain long-lasting flame retardant property. The product is high in washing resistance after being applied to the fabric and is ecological, environmentally friendly and convenient to use, and the colored light and handfeel of the fabric are hardly influenced.

Description

technical field

[0001] The invention relates to the field of flame retardant and its synthesis and preparation, in particular to a s-triazine type flame retardant, its preparation method and its application in the preparation of natural fibers. Background technique

[0002] In today's society, the global fire situation is very serious. In recent years, fires have occurred frequently in China, which poses a serious threat to the safety of human life and property. In order to prevent the occurrence of fire, in addition to taking fire prevention measures, textiles with flame retardant properties can also be used. However, many flame retardants currently face problems such as poor flame retardant effect, low mechanical strength, and poor washing limit oxygen index (LOI). The application of flame retardants is limited.

[0003] At present, my country's flame-retardant finishing of textiles is still in the initial stage of exploration. Halogen-based and boron-based flame retarda...

Examples

Embodiment 1

[0043] Step 1: Full dissolution of cyanuric chloride

[0044] In a 500ml four-necked flask equipped with a stirrer and a thermometer, add 8g (0.043mol) of cyanuric chloride and 250ml (196.13g) of acetone to fully dissolve to obtain a base liquid.

[0045] Step 2: Preparation of s-triazine flame retardant

[0046] Move the above base liquid to a temperature of 0°C, and continuously add 15.90 g (0.0946 mol) of diethyl hydroxymethyl phosphate to the base liquid, and the addition is completed in 1 hour; Potassium aqueous solution adjusts pH=5. At different stages of the reaction, draw a small amount of reaction solution, and use thin-layer chromatographic analysis to determine whether the reaction of cyanuric chloride is complete. After the diethyl hydroxymethyl phosphate has been added dropwise, move to room temperature at 25°C for 35 minutes until cyanuric chloride disappears.

[0047] The concrete reaction formula of this step is as follows:

[0048]

[0049] Step 3: Pur...

Embodiment 2

[0057] Step 1: Full dissolution of cyanuric chloride

[0058] In a 500ml four-neck flask equipped with a stirrer and a thermometer, add 8g (0.043mol) of cyanuric chloride and 200ml (156.9g) of acetone to fully dissolve to obtain a base solution.

[0059] Step 2: Preparation of s-triazine flame retardant

[0060] Move the above base liquid to a temperature of -5°C, and continuously add 15.13g (0.090mol) of diethyl hydroxymethyl phosphate to the base liquid dropwise, and the dropwise addition is completed in 1 hour; during this period, 5% by mass of Potassium carbonate aqueous solution adjusts pH=6. At different stages of the reaction, draw a small amount of reaction solution, and use thin-layer chromatographic analysis to determine whether the reaction of cyanuric chloride is complete. After the diethyl hydroxymethyl phosphate has been added dropwise, move to room temperature at 25°C for 30 minutes until cyanuric chloride disappears.

[0061] The concrete reaction formula of...

Embodiment 3

[0067] Step 1: Full dissolution of cyanuric chloride

[0068] In a 500ml four-necked flask equipped with a stirrer and a thermometer, add 8g (0.043mol) of cyanuric chloride and 300ml (235.35g) of acetone to fully dissolve to obtain a base liquid.

[0069] Step 2: Preparation of s-triazine flame retardant

[0070] Move the above base liquid to a temperature of 5°C, and continuously add 14.46g (0.086mol) of diethyl hydroxymethyl phosphate to the base liquid dropwise, and the dropwise addition is completed in 1 hour; Potassium aqueous solution adjusts pH=7. At different stages of the reaction, draw a small amount of reaction solution, and use thin-layer chromatographic analysis to determine whether the reaction of cyanuric chloride is complete. After the diethyl hydroxymethyl phosphate has been added dropwise, move to room temperature at 25°C for 40 minutes until cyanuric chloride disappears.

[0071] The concrete reaction formula of this step is as follows:

[0072]

[00...

technical field

[0001] The invention relates to the field of flame retardant and its synthesis and preparation, in particular to a s-triazine type flame retardant, its preparation method and its application in the preparation of natural fibers. Background technique

[0002] In today's society, the global fire situation is very serious. In recent years, fires have occurred frequently in China, which poses a serious threat to the safety of human life and property. In order to prevent the occurrence of fire, in addition to taking fire prevention measures, textiles with flame retardant properties can also be used. However, many flame retardants currently face problems such as poor flame retardant effect, low mechanical strength, and poor washing limit oxygen index (LOI). The application of flame retardants is limited.

[0003] At present, my country's flame-retardant finishing of textiles is still in the initial stage of exploration. Halogen-based and boron-based flame retarda...

Examples

Embodiment 1

[0043] Step 1: Full dissolution of cyanuric chloride

[0044] In a 500ml four-necked flask equipped with a stirrer and a thermometer, add 8g (0.043mol) of cyanuric chloride and 250ml (196.13g) of acetone to fully dissolve to obtain a base liquid.

[0045] Step 2: Preparation of s-triazine flame retardant

[0046] Move the above base liquid to a temperature of 0°C, and continuously add 15.90 g (0.0946 mol) of diethyl hydroxymethyl phosphate to the base liquid, and the addition is completed in 1 hour; Potassium aqueous solution adjusts pH=5. At different stages of the reaction, draw a small amount of reaction solution, and use thin-layer chromatographic analysis to determine whether the reaction of cyanuric chloride is complete. After the diethyl hydroxymethyl phosphate has been added dropwise, move to room temperature at 25°C for 35 minutes until cyanuric chloride disappears.

[0047] The concrete reaction formula of this step is as follows:

[0048]

[0049] Step 3: Pur...

Embodiment 2

[0057] Step 1: Full dissolution of cyanuric chloride

[0058] In a 500ml four-neck flask equipped with a stirrer and a thermometer, add 8g (0.043mol) of cyanuric chloride and 200ml (156.9g) of acetone to fully dissolve to obtain a base solution.

[0059] Step 2: Preparation of s-triazine flame retardant

[0060] Move the above base liquid to a temperature of -5°C, and continuously add 15.13g (0.090mol) of diethyl hydroxymethyl phosphate to the base liquid dropwise, and the dropwise addition is completed in 1 hour; during this period, 5% by mass of Potassium carbonate aqueous solution adjusts pH=6. At different stages of the reaction, draw a small amount of reaction solution, and use thin-layer chromatographic analysis to determine whether the reaction of cyanuric chloride is complete. After the diethyl hydroxymethyl phosphate has been added dropwise, move to room temperature at 25°C for 30 minutes until cyanuric chloride disappears.

[0061] The concrete reaction formula of...

Embodiment 3

[0067] Step 1: Full dissolution of cyanuric chloride

[0068] In a 500ml four-necked flask equipped with a stirrer and a thermometer, add 8g (0.043mol) of cyanuric chloride and 300ml (235.35g) of acetone to fully dissolve to obtain a base liquid.

[0069] Step 2: Preparation of s-triazine flame retardant

[0070] Move the above base liquid to a temperature of 5°C, and continuously add 14.46g (0.086mol) of diethyl hydroxymethyl phosphate to the base liquid dropwise, and the dropwise addition is completed in 1 hour; Potassium aqueous solution adjusts pH=7. At different stages of the reaction, draw a small amount of reaction solution, and use thin-layer chromatographic analysis to determine whether the reaction of cyanuric chloride is complete. After the diethyl hydroxymethyl phosphate has been added dropwise, move to room temperature at 25°C for 40 minutes until cyanuric chloride disappears.

[0071] The concrete reaction formula of this step is as follows:

[0072]

[00...

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