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Reactive phosphorus flame retardant and preparation method thereof

A phosphorus-based flame retardant and reactive technology, which is applied in the field of reactive phosphorus-based flame retardants and their preparation, can solve the problem of less halogen-free flame retardants, and achieve the effects of improved toughness, high purity, and easy control

Inactive Publication Date: 2016-04-13
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are very few varieties of halogen-free flame retardants that can be applied to the market at present, and it is urgent to develop new products suitable for industrialization

Method used

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  • Reactive phosphorus flame retardant and preparation method thereof
  • Reactive phosphorus flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Step 1: Add PEPA16.24g and phosphorus oxychloride 5ml into a 250ml three-necked flask equipped with a reflux condenser, a thermometer and a magnet, then add 50ml of acetonitrile as a solvent, and raise the reaction temperature until the temperature rises to 80°C. The catalyst DMAP is added, and the reaction temperature is controlled between 80-82°C. After continuing the reaction for 25 hours, a white solid precipitates out. After the product is washed with acetone or acetonitrile, the white powder obtained after drying at 60°C is the intermediate.

[0028] Step 2: Add 2.63g of intermediates and 1.53g of polyethylene glycol to a 100ml three-necked flask equipped with a reflux condenser, thermometer and magnet, and then add 40ml of acetonitrile as a solvent. After the temperature rises to 80°C, add 0.1g of DMAP In the three-necked flask, control the temperature at 80-82°C for reaction. After 25 hours of reaction time, the temperature was lowered to room temperature, and a...

Embodiment 2

[0031] The first step: the synthesis method of a reactive phosphorus-based flame retardant intermediate is the same as in Example 1.

[0032] Step 2: Add 2.60g of intermediates and 1.7g of polyethylene glycol to a 100ml three-necked flask equipped with a reflux condenser, thermometer and magnet, and then add 25ml of DMSO as a solvent. After the temperature rises to 80°C, add an acid-binding agent: 0.52g pyridine; then add catalyst: 0.1g DMAP was added into the three-necked flask, and the temperature was controlled to react at 80-82°C. After 20 hours of reaction time, it was lowered to room temperature to obtain a yellow solution and a precipitate, which were suction filtered, washed and dried to obtain a white solid powder.

[0033] Step 3: Step 3: Add 4.31g of polymer and 0.75g of epichlorohydrin to a 100ml three-necked flask equipped with a magnetic stirrer, a thermometer and a magnet. After heating up to 90°C, add 0.1g of DMAP and 0.50g of pyridine Add it into a three-neck...

Embodiment 3

[0035] The first step: the synthesis method of a reactive phosphorus-based flame retardant intermediate is the same as in Example 1.

[0036] Step 2: Add 2.55g of intermediates and 1.8g of polyethylene glycol to a 100ml three-necked flask equipped with a reflux condenser, thermometer and magnet, and then add 30ml of DMSO as a solvent. After the temperature rises to 90°C, add an acid-binding agent: 0.71g triethylamine; then add catalyst: 0.1g DMAP is added into the three-necked flask, and the temperature is controlled at 90-95°C for reaction. After 25 hours of reaction time, it was lowered to room temperature to obtain a yellow solution and a precipitate, which were suction filtered, washed and dried to obtain a white solid powder.

[0037] Step 3: Add 4g of polymer and 0.8g of epichlorohydrin to a 100ml three-necked flask equipped with a magnetic stirrer, a thermometer and a magnet. After the temperature rises to 90°C, add 0.1g of DMAP and 0.72g of triethylamine to the three-n...

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Abstract

Te invention relates to a synthetic flame retardant and a preparation method thereof, and concretely relates to a reactive phosphorus flame retardant and a preparation method thereof. Preparation raw materials used in the invention comprise PEPA (1-oxyphospha-4-hydroxymethyl-2,6,7-trioxabicyclo[2.2.2]octane), phosphorous oxychloride (POCl3), polyethylene glycol and chloropropylene oxide. The preparation method of the flame retardant comprises the following steps: 1, reacting the PEPA with phosphorous oxychloride under certain conditions to generate an intermediate; 2, reacting the synthesized intermediate with polyethylene glycol under certain conditions to generate a new polymer; and 3, reacting chloropropylene oxide with the polymer to generate a final product, filtering the product, washing the filtered product, and drying the washed product to obtain a white solid. The phosphorus content of the above disclosed product is 10% or above, and the compound has good flame retardation performance. The preparation method of the product has the advantages of simplicity, simple post-treatment and development potential.

Description

technical field [0001] The invention relates to a phosphorus-based flame retardant and a preparation method thereof, in particular to a reactive phosphorus-based flame retardant and a preparation method thereof. Background technique [0002] With the wide application of polymer materials in daily life, the inherent problems have also been exposed. Since the 1950s, polymer materials and their products based on plastics, rubber, fibers and other synthetic materials The fire accidents caused by its flammability have caused heavy casualties and property losses to the society. Flame-retardant polymer materials have the characteristics of being difficult to ignite and self-extinguishing when away from the fire. Even if it catches fire, it will slow down the spread of the flame, which can prevent a small fire from developing into a catastrophic fire, giving people more time to evacuate or extinguish fire, thereby reducing the risk of fire hazards. [0003] Therefore, research on ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/337C08L71/02
CPCC08G65/337C08L71/02C08L2201/02C08L2201/22
Inventor 梁兵修力轩
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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