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Preparation method of viscose fiber co-soluble hydroxyl thiophosphate flame retardant

A technology of hydroxyphosphorothioate and viscose fiber, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., and can solve the problem of low economic benefit, insufficient reaction, trichlor Oxyphosphorus volatilization and other problems, to achieve the effect of safe operation, simple process and convenient operation

Active Publication Date: 2021-07-16
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0017] The Sandoflame5060 viscose fiber flame retardant produced by the Swiss Sandoz Company, because the more the product is, the more difficult it is to stir, and mechanical stirring is required. However, the solvent is easy to evaporate along the gap under heating conditions, so it is necessary to continuously add solvent; Tokuyasu needs to first React with water to generate acid and then react with alcohols; Xingyi Wang’s reactant, phosphorus pentoxide, will agglomerate after a period of time, cannot fully react, and needs to be ground; Zhang Shengqiang’s preparation of DOPNP requires two steps to complete, and the reaction time is long , the economic benefit is not high; Denghui Wu reacted with excess phosphorus oxychloride in the first step, and heating caused the volatilization of phosphorus oxychloride, resulting in waste

Method used

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  • Preparation method of viscose fiber co-soluble hydroxyl thiophosphate flame retardant
  • Preparation method of viscose fiber co-soluble hydroxyl thiophosphate flame retardant
  • Preparation method of viscose fiber co-soluble hydroxyl thiophosphate flame retardant

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044]Add a magnetic stirrer to the 500mL three-necked flask, install a thermometer, and a constant pressure dropping funnel, add neopentyl glycol (10.4g, 0.1mol), phosphorus trichloride (16.9g, 0.1mol), cyclohexane (200mL), Use an ice-salt bath to keep the reaction temperature below 0 degrees Celsius, slowly add triethylamine (28mL, 0.2mol) dropwise, after the dropwise addition, react at room temperature for 2-4h; continue to add erythritol (6.1g, 0.05mol ) and triethylamine (21mL, 0.15 mol), heated to reflux for 6-8h. The product was neutralized to neutral with 10% sodium hydroxide solution, stirred at room temperature for 30 min and suction filtered to obtain a solid, washed with cold water and absolute ethanol, and dried to obtain a white solid (1,4-bis(5,5-di Methyl-2-thiophospha-1,3-dioxan-2-oxyl)-2,3-butanediol) 17.11 g, yield: 76%. 1 H NMR (600MHz, DMSO) δ: 4.33 (dd, J = 10.4, 3.2Hz, 4H, -CH 2 O), 4.15 (dd, J=29.1, 11.0 Hz, 4H, -CH 2 O), 3.91(d, J=12.0Hz, 8H, -CH 2...

Embodiment 2

[0046] Add a magnetic stirrer to the 500mL three-necked flask, install a thermometer, and a constant pressure dropping funnel, add neopentyl glycol (10.4g, 0.1mol), phosphorus trichloride (16.9g, 0.1mol), cyclohexane (200mL), Use an ice-salt bath to keep the reaction temperature below 0 degrees Celsius, slowly add triethylamine (35mL, 0.25mol) dropwise, after the dropwise addition, react at room temperature for 2-4h; continue to add erythritol (6.1g, 0.05mol ) and triethylamine (21mL, 0.15mol), heated to reflux for 6-8h. The product was neutralized to neutral with 10% sodium hydroxide solution, stirred at room temperature for 30 minutes to obtain a solid by suction filtration, washed with cold water and absolute ethanol, and dried to obtain 17.57 g of white solid, yield: 78%.

Embodiment 3

[0048] Add a magnetic stirrer to the 500mL three-necked flask, install a thermometer, and a constant pressure dropping funnel, add neopentyl glycol (10.4g, 0.1mol), phosphorus trichloride (16.9g, 0.1mol), cyclohexane (200mL), Use an ice-salt bath to keep the reaction temperature below 0°C, slowly add triethylamine (41mL, 0.29mol) dropwise, after the dropwise addition, react at room temperature for 2-4h; continue to add erythritol (6.1g, 0.05mol ) and triethylamine (21mL, 0.15mol), heated to reflux for 6-8h. The product was neutralized to neutral with 10% sodium hydroxide solution, stirred at room temperature for 30 minutes and suction filtered to obtain a solid, washed with cold water and absolute ethanol, and dried to obtain 18.02 g of white solid, yield: 80%.

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Abstract

The invention discloses a preparation method of a viscose fiber co-soluble hydroxyl thiophosphate flame retardant, which belongs to the technical field of organic synthesis. The method comprises the following steps of by taking neopentyl glycol and thiophosphoryl chloride as raw materials, maintaining the reaction temperature below 0 DEG C by using an ice salt bath, slowly dropwise adding triethylamine, and reacting at room temperature after dropwise adding, continuously adding erythritol and triethylamine, and heating and refluxing, and neutralizing the reaction solution to be neutral by using a 10% sodium hydroxide solution, stirring at room temperature, performing suction filtration to obtain a solid, washing with cold water and absolute ethyl alcohol, and performing suction drying to obtain a white solid. According to the method, the 1, 4-bis(5, 5-dimethyl-2-thiophosphoryl-1, 3-dioxane-2-oxy)-2, 3-butanediol is prepared under conventional conditions, an intermediate does not need to be separated and purified, the operation is safe and simple, and energy is saved. The method has the advantages of cheap initial raw materials and reduction of the production cost. The method is simple in process, low in energy consumption, convenient to operate and suitable for industrial large-scale production.

Description

technical field [0001] The invention relates to a viscose fiber co-soluble hydroxy phosphorothioate flame retardant: 1,4-bis(5,5-dimethyl-2-thiophospha-1,3-dioxane-2 The preparation method of -oxygen)-2,3-butanediol belongs to the technical field of organic synthesis. Background technique [0002] 1,4-bis(5,5-dimethyl-2-thiophospha-1,3-dioxane-2-oxyl)-2,3-butanediol is a flame retardant based on Sandoflame 5060 A viscose fiber co-soluble hydroxy phosphorothioate flame retardant designed, which is directly mixed with alkali cellulose during use, reacts with carbon disulfide to form xanthate, forms viscose, and is spun into acid to form viscose The glue fiber makes the flame retardant molecules and the viscose fiber molecules mix at the molecular level, so as to realize the high-efficiency flame retardancy of the viscose fiber. [0003] 1,4-bis(5,5-dimethyl-2-thiophospha-1,3-dioxane-2-oxyl)-2,3-butanediol molecular formula is C 14 h 28 o 8 P 2 S 2 , whose chemical formu...

Claims

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Application Information

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IPC IPC(8): C07F9/6574
CPCC07F9/65742
Inventor 高欣钦李学芬俞鸿博王荣炎张硕
Owner DALIAN UNIV OF TECH