Method for preparing phosphorus-containing organosilicon flame retardant

A flame retardant and organosilicon technology, which is applied in the field of preparation of phosphorus-containing organosilicon flame retardants, can solve problems such as poor stability and environmental impact, and achieve the effect of good stability and simple technical route

Active Publication Date: 2011-01-05
江苏金石电力设计有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the strong activity of phosphorus oxychloride reaction, it is easy to hydrolyze and has poor stability, and when it reacts with amino groups, it will produce HCl by-products, which will easily affect the environment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A 250ml three-necked bottle is equipped with a stirrer, a thermometer and a distillation device, and 2.5g of triethylamine, 79.9g (0.01 mol) of hydroxymethyl silicone resin (the structural formula is Me 3 SiO(Me 2 SiO) 40 (MeHOSiO) 20 (MeSiO 3 / 2 ) 50 SiMe 3 , the number of hydroxyl moles is 0.2) and 36.4g (0.2mol) of triethyl phosphate, stirred and mixed, and reacted at 80°C for 20h. Filtration and steaming to remove low boilers gave 101.7g of phosphorus-containing organosilicon flame retardant with a yield of 95%.

[0028] Flame retardant application performance: Put ABS and the prepared phosphorus-containing silicone flame retardant into a high-speed mixer at a weight ratio of 85:15, mix at high speed for 3 minutes, and discharge for later use. The high-speed kneaded raw materials were extruded on a twin-screw extruder, and the extruded melt was vacuum-dried at 100 °C for 6 h, then pressed on an automatic film laminator, and demolded to obtain samples. The oxy...

Embodiment 2

[0030] A 1000ml three-necked bottle is equipped with a stirrer, a thermometer and a distillation device, and 15g of sodium hydroxide, 700g (0.1mol) of hydroxymethylphenyl silicone resin (the structural formula is Me 3 SiO(Me 2 SiO) 20 (MeHOSiO) 10 (PhHOSiO) 10 (MeSiO 3 / 2 ) 48 SiMe 3 , the molar number of hydroxyl groups is 2.0) and 12.4g (0.1mol) of trimethyl phosphite, stirred and mixed, reacted at 130°C for 4h, filtered, and evaporated to remove low boilers to obtain 674.7g of phosphorus-containing organosilicon flame retardant. The yield was 96%.

[0031]Flame retardant application performance: The prepared phosphorus-containing silicone flame retardant and polypropylene are mixed in a ratio of 30:70, and the sample is extruded in a single-screw extruder. The oxygen index of the sample tested by an oxygen index meter reaches 29.20%, and the oxygen index of polypropylene without flame retardant is 18.5%. The vertical combustion test of the sample was carried out with...

Embodiment 3

[0033] A 1000ml three-necked bottle is equipped with a stirrer, a thermometer and a distillation device, and 20g of dibutyltin dilaurate, 340g (0.01mol) of hydroxymethyl silicone resin (the structural formula is HOMe 2 SiO(MeHOSiO) 40 (MeSiO 3 / 2 ) 440 (HOSiO 3 / 2 ) 10 SiMe 3 , the molar number of hydroxyl groups is 0.5), 240g (0.01mol) containing hydroxymethyl phenyl silicone resin (the structural formula is Me 3 SiO(Me 2 SiO) 20 (MeHOSiO) 70 (PhSiO 3 / 2 ) 100 (SiO 2 ) 70 SiMe 3 The molar number of hydroxyl groups is 0.7), 26.6g (0.1mol) of tributyl phosphate and 16.6g (0.1mol) of triethyl phosphite, stirred and mixed, reacted at 150°C for 15h, filtered, and evaporated to remove low boilers to obtain 552.2g of phosphorus-containing silicone flame retardant. The yield was 94%.

[0034] Flame retardant application performance: After mixing PC and the prepared phosphorus-containing silicone flame retardant in a ratio of 75:25, extrude and pelletize in a twin-screw e...

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Abstract

The invention relates to a method for preparing a phosphorus-containing organosilicon flame retardant, and provides a method for preparing a phosphorus-containing flame retardant, which has the advantages of rich raw materials, low cost, simple production technology, no HCl generated in a reaction, and recyclable by-products of the reaction to solve the technical problems. The preparation process comprises the following steps of: reacting an active phosphorus compound with a hydroxyl-containing polysiloxane in the presence of a catalyst, wherein the molar ratio of the active phosphorus compound to the hydroxyl-containing polysiloxane is 1:1-20; and after the reaction, filtering, and steaming to remove low-boiling-point substances to obtain the product of the phosphorus-containing organosilicon flame retardant.

Description

technical field [0001] The invention relates to the technical field of flame retardant synthesis, in particular to a method for preparing a phosphorus-containing organosilicon flame retardant. The phosphorus-containing silicone flame retardant can be used as a flame retardant in polyolefin, polycarbonate, ABS, nylon, and PC / ABS. Compared with traditional flame retardants, it is highly efficient and low-toxic, and is an environmentally friendly type flame retardant. Background technique [0002] With the development of my country's synthetic material industry and the continuous expansion of application fields, flame retardants have broad market prospects in various fields such as chemical building materials, electronic appliances, transportation, aerospace, daily furniture, interior decoration, and basic necessities of life. [0003] Organophosphorus flame retardant is a kind of flame retardant with good flame retardant performance. It has dual functions of flame retardant a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/395C08L23/00C08L69/00C08L55/02C08L77/00C08L83/08
Inventor 来国桥李美江蒋剑雄倪勇邓元
Owner 江苏金石电力设计有限公司
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