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A kind of reactive phosphorus flame retardant and preparation method thereof

A phosphorus-based flame retardant and a reactive technology, which are applied in the field of reactive phosphorus-based flame retardants and their preparation, can solve the problem of less halogen-free flame retardants and the like, achieve improved toughness, simple preparation method, and improved easy hydrolysis Effect

Inactive Publication Date: 2017-12-01
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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  • A kind of reactive phosphorus flame retardant and preparation method thereof
  • A kind of reactive phosphorus flame retardant and preparation method thereof
  • A kind of reactive phosphorus flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Step 1: Add 16.24 g of PEPA and 5 ml of phosphorus oxychloride to a 250 ml three-necked flask equipped with a reflux condenser, a thermometer and a magnet, then add 50 ml of solvent acetonitrile, and raise the reaction temperature until the temperature rises to 80 ℃, add the catalyst DMAP, control the reaction temperature between 80-82 ℃, after 25 hours of continuous reaction, a white solid precipitates, the product is washed with acetone or acetonitrile, and the white powder obtained after drying at 60 ℃ is the intermediate.

[0030] Step 2: Add 2.63 g of intermediates and 1.53 g of polyethylene glycol to a 100 ml three-neck flask equipped with a reflux condenser, a thermometer and a magnet, and then add 40 ml of acetonitrile as a solvent. g DMAP was added to the three-necked flask, and the temperature was controlled to react at 80-82 °C. After 25 h of reaction time, the temperature was lowered to room temperature, and a white precipitate was obtained, which was suctio...

Embodiment 2

[0033] The first step: the synthesis method of a reactive phosphorus-based flame retardant intermediate is the same as in Example 1.

[0034] Step 2: Add 2.60 g of intermediates and 1.7 g of polyethylene glycol to a 100 ml three-necked flask equipped with a reflux condenser, a thermometer and a magnet, and then add 25 ml of DMSO as a solvent. After the temperature rises to 80 °C, add Acid agent: 0.52 g pyridine; add catalyst: 0.1 g DMAP into the three-necked flask, and control the temperature at 80-82 °C for reaction. After the reaction time was 20 h, it was lowered to room temperature, and a yellow solution and a precipitate were obtained, which were suction filtered, washed, and dried to obtain a white solid powder.

[0035] Step 3: Step 3: Add 4.31 g of polymer and 0.75 g of epichlorohydrin to a 100 ml three-neck flask equipped with a magnetic stirrer, a thermometer, and a magnet. After heating up to 90 °C, add 0.1 g of DMAP and 0.50 g pyridine was added into the three-nec...

Embodiment 3

[0037] The first step: the synthesis method of a reactive phosphorus-based flame retardant intermediate is the same as in Example 1.

[0038] Step 2: Add 2.55 g of intermediates and 1.8 g of polyethylene glycol to a 100 ml three-neck flask equipped with a reflux condenser, a thermometer and a magnet, and then add 30 ml of DMSO as a solvent. After the temperature rises to 90 °C, add Acid agent: 0.71 g triethylamine; Add catalyst: 0.1 g DMAP into the three-necked flask, control the temperature at 90-95 °C for reaction. After 25 h 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.

[0039] Step 3: Add 4 g of polymer and 0.8 g of epichlorohydrin to a 100 ml three-necked flask equipped with a magnetic stirrer, a thermometer, and a magnet. After heating up to 90 °C, add 0.1 g of DMAP and 0.72 g of triethylamine Add it into a three-necked flask, and control ...

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Abstract

A reactive phosphorus-based flame retardant and a preparation method thereof, relating to a synthetic flame retardant and a preparation method thereof, the preparation raw materials include: PEPA (1-oxyphospha-4-hydroxymethyl-2,6,7 ‑trioxabicyclo[2.2.2]octane), phosphorus oxychloride (POCl3), polyethylene glycol and epichlorohydrin. The steps for preparing the flame retardant are divided into three steps. The first step is to react PEPA and phosphorus oxychloride under certain conditions to form an intermediate; the second step is to combine the synthesized intermediate and Polyethylene glycol reacts under certain conditions to form a new polymer. Step 3: Epichlorohydrin reacts with the polymer to form the final product. The product was filtered, washed and dried to obtain a white solid. The phosphorus content of the compound is more than 10%, and it has good flame retardant properties. The production process of this product is simple, the aftertreatment is convenient and convenient, and it has 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 been exposed. Since the 1950s, polymer materials and their products mainly composed of 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, researc...

Claims

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Application Information

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Patent Type & Authority Patents(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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