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Halogen-free phosphorus-containing flame retardant, preparation method thereof and bio-based halogen-free flame-retardant polylactic acid material prepared from halogen-free phosphorus-containing flame retardant

A technology of flame retardant and polylactic acid, which is applied in the manufacture of fire-retardant and flame-retardant filaments, chemical instruments and methods, compounds of elements of Group 5/15 of the periodic table, etc. , material performance reduction and other issues, to achieve the effect of high flame retardant efficiency, reduced mechanical properties, and extended service life

Pending Publication Date: 2020-08-04
马德里高等材料研究院 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These flame-retardant polylactic acid modification methods have problems such as residual organic solvents, excessive addition of flame retardants, difficulty in molding PLA in the process, and reduced material properties.

Method used

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  • Halogen-free phosphorus-containing flame retardant, preparation method thereof and bio-based halogen-free flame-retardant polylactic acid material prepared from halogen-free phosphorus-containing flame retardant
  • Halogen-free phosphorus-containing flame retardant, preparation method thereof and bio-based halogen-free flame-retardant polylactic acid material prepared from halogen-free phosphorus-containing flame retardant
  • Halogen-free phosphorus-containing flame retardant, preparation method thereof and bio-based halogen-free flame-retardant polylactic acid material prepared from halogen-free phosphorus-containing flame retardant

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Experimental program
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Embodiment approach

[0087] According to a preferred embodiment of the present invention, the amino alcohol compound is NH 2 C(CH 2 Oh) 2 (CH 2 ) n (CH 2 OH) or NH 2 (CH 2 CHOH) m CH 3 , wherein, n is an integer of 0-6, and m is an integer of 1-10.

[0088] According to a particularly preferred embodiment of the present invention, the aminoalcohol compound is aminobutanol (NH 2 C(CH 2 Oh) 3 ) or aminoisopropanol (NH 2 (CH 2 CHOH)CH 3 ), that is, n is 0 and m is 1.

[0089] According to another preferred embodiment of the present invention, the aminophenol compound is selected from 2-aminophenol is preferred 3-Aminophenol or 4-aminophenol That is, n is 0.

[0090] The second aspect of the present invention provides a halogen-free phosphorus-containing flame retardant, which is prepared from phytic acid and aminoalcohol or aminophenol compounds, preferably phytic acid and aminoalcohol compounds.

[0091] According to the present invention, the halogen-free phosphorus-containi...

Embodiment 1

[0162] Embodiment 1 Preparation of phytic acid-tromethamine halogen-free phosphorus-containing flame retardant

[0163] Dissolve 60 mmol of tromethamine in ethanol solvent, then slowly drop 5 mmol of phytic acid into the ethanol solution of tromethamine, monitor the pH value of the solution throughout the reaction until the solution is neutral, and end the reaction.

[0164] The precipitated product was collected and dried in a vacuum oven: first dried at 80° C. for 2 hours and then at 150° C. for 1 hour to obtain a phytic acid-tromethamine halogen-free phosphorus-containing flame retardant.

[0165] Infrared test (Nicolet iS50 Fourier transform infrared spectrometer) is carried out to gained phytic acid-tromethamine halogen-free phosphorus flame retardant, gained test result is as follows figure 1 shown.

[0166] figure 1 Among them, curve a is the infrared curve of tromethamine, curve b is the infrared curve of phytic acid, and curve c is the infrared curve of phytic acid-...

Embodiment 2

[0176] Embodiment 2 Preparation of phytic acid-aminoisopropanol halogen-free phosphorus-containing flame retardant

[0177] Dissolve 60mmol of aminoisopropanol in ethanol solvent, then slowly drop 5mmol of phytic acid into the ethanol solution of aminoisopropanol, monitor the pH value of the solution throughout the reaction until the solution is neutral, and end the reaction.

[0178] The precipitated product was collected and dried in a vacuum oven: dried at 80° C. for 2 hours, and dried at 150° C. for 1 hour to obtain a phytic acid-aminoisopropanol halogen-free phosphorus-containing flame retardant.

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Abstract

The invention discloses a halogen-free phosphorus-containing flame retardant and a preparation method thereof. The halogen-free phosphorus-containing flame retardant has a structural general formula described in the specification, wherein -R1 to R12 are selected from one or more of alcoholic amino groups or phenolic amino groups, and the halogen-free phosphorus-containing flame retardant integrates a bio-based acid source and a carbon source, and is high in flame retardant efficiency, simple in synthesis process, pollution-free, green and environment-friendly in raw materials and low in cost.The invention also discloses a bio-based halogen-free flame-retardant polylactic acid material prepared from the flame retardant. The bio-based halogen-free flame-retardant polymerized emulsion with excellent flame-retardant property and better mechanical property is obtained by adding a small amount of the flame retardant and optionally adding a flame retardant aid and an antioxidant. When the addition amount of the flame retardant accounts for 0.5-8.9% of the mass fraction of polylactic acid, the limit oxygen index of the obtained bio-based halogen-free flame-retardant polylactic acid reaches 24-33%. The preparation method of the bio-based halogen-free flame-retardant polylactic acid material is simple, free of solvent influence, easily available in raw materials, easily controllable intechnological process and suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of flame retardants and flame retardant polymers, and in particular relates to a halogen-free phosphorus-containing flame retardant, a preparation method thereof, and a bio-based halogen-free flame-retardant polylactic acid material used for the preparation. Background technique [0002] Compared with other polymer materials, polylactic acid (PLA) from bio-based sources is increasingly used in engineering, It is an ideal green material and has broad market prospects. [0003] However, the innate flammability of polylactic acid limits its wider use to a large extent, specifically including that the vertical combustion test has no grades and the limiting oxygen index (LOI) is only about 20%, so improving the flame retardancy of polylactic acid is an urgent need. work around. Among them, adding flame retardants is a commonly used and effective method in the processing of polylactic acid. [0004] There are two kinds o...

Claims

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Application Information

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IPC IPC(8): C08K5/5399C08L67/04C08K5/00C08K5/134C08K5/526D01F6/92D01F1/07C07F9/24
CPCC07F9/2416C08K5/00C08K5/1345C08K5/526C08K5/5399C08L2201/02C08L2201/08C08L2201/22D01F1/07D01F6/92C08L67/04
Inventor 王德义杨云仙王锐张秀芹张安莹
Owner 马德里高等材料研究院
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