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Polymeric phosphorus-nitrogen-silicon flame retardant as well as synthesis method and application thereof

A synthesis method, the technology of phosphorus nitrogen and silicon, which is applied in the field of flame retardants, can solve the problems such as the absence of polymeric phosphorus nitrogen and silicon flame retardants, and achieve the effects of excellent flame retardancy and improved impact resistance

Inactive Publication Date: 2019-02-15
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] However, polymeric phosphorus nitrogen silicon flame retardants have not been reported in the literature

Method used

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  • Polymeric phosphorus-nitrogen-silicon flame retardant as well as synthesis method and application thereof
  • Polymeric phosphorus-nitrogen-silicon flame retardant as well as synthesis method and application thereof
  • Polymeric phosphorus-nitrogen-silicon flame retardant as well as synthesis method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Step 1: the synthesis of PEPA, the synthetic route is as follows:

[0032]

[0033] Specifically: add 0.50 mol of pentaerythritol and 240 mL of 1,4-dioxane into a 500 mL four-necked flask equipped with nitrogen protection, a mechanical stirrer, a thermometer, a spherical condenser, and a tail gas absorption device. Access to N 2 , heated and stirred to raise the temperature to 70°C. When the temperature of the reaction system rose to 70°C and the pentaerythritol was partially dissolved, 0.55mol of phosphorus oxychloride was started to be added dropwise, and the dropwise addition was completed within 2 hours. After the dropwise addition, keep warm for 20 minutes, then raise the temperature until the system refluxes, keep warm for 6 hours, until no obvious white smoke is produced in the tail gas absorption device. After the reaction was completed, it was allowed to stand overnight, filtered with suction, and the filter cake was washed twice with solvents 1,4-dioxane a...

Embodiment 2

[0041] This example is basically the same as Example 1, except that the molar ratio of PDCP to 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane is 0.8: 1. The final yield was 83%, lower than Example 1.

Embodiment 3

[0047] 1. Use the SX2-25-10 box-type resistance furnace produced by Shanghai Experimental Instrument Factory to test the sample, dry the PNSFR in the oven at 100°C for about 2 hours, and then accurately weigh 1.0g of PNSFR with an analytical balance and put it Put the crucible into the crucible, put the crucible into a box-type resistance furnace for calcination at 500°C for 30 minutes, take it out after cooling, use an analytical balance to accurately measure the expansion volume and carbon residue after calcination, and finally calculate the expansion degree and carbon residue by calculation formula quantity. The calculation formula is as follows:

[0048]

[0049]

[0050] The above are the calculation formulas of expansion degree and carbon residue amount, where ID and R are expansion degree and carbon residue rate respectively, ΔV is the volume change of the sample before and after calcination, M is the product quality before calcination, and m is the product qualit...

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Abstract

The invention discloses a polymeric phosphorus-nitrogen-silicon flame retardant as well as a synthesis method and application thereof. The structural formula of the polymeric phosphorus-nitrogen-silicon flame retardant is shown in the description. An intermediate polydichlorophosphazene (PDCP) is formed from pentaerythritol octahydrogen tetraphosphate (PEPA) and triphosphoyl chloride via nucleophilic substitution, and reacts with a silicone monomer 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyl disiloxane for forming the polymeric phosphorus-nitrogen-silicon flame retardant. The flame retardant provided by the invention integrates the three components of phosphorus, nitrogen and silicon into one molecule, has abilities of carbonization, foaming, oxygen insulation, heat insulation, inhibition to material degradation, and the like, plays a synergistic effect, has high content of Si and obviously improves a base material in mechanical properties such as impact resisting property, tensile property, and the like.

Description

technical field [0001] The invention belongs to the technical field of flame retardants, and relates to a polymeric phosphorus nitrogen silicon flame retardant, a synthesis method and an application thereof. Background technique [0002] Flame retardant, as a functional additive to improve the flame retardancy, self-extinguishing or smoke suppression of flammable or combustible materials, is one of the main additives for important fine chemical products and synthetic materials. Social security is very important, and it is widely used in many fields such as daily necessities, electronic appliances, transportation, defense industry, aerospace industry and construction. Halogen flame retardants have the advantages of good flame retardant effect, less dosage, and little impact on the mechanical properties of materials. They have been used as the main flame retardant for a long time, but the processed materials will produce toxic and corrosive gases when they are heated and burne...

Claims

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Application Information

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IPC IPC(8): C08G79/02C08L85/02C08L77/06
CPCC08G79/02C08L77/06C08L2201/02C08L85/02
Inventor 霍雅洁刘煜炜夏静朱广军罗闯
Owner NANJING UNIV OF SCI & TECH
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