Surface treatment of natural magnesium hydroxide Influence on properties of HFFR cable compounds
2024-05-27

Incorporating high amount of mineral filler into a thermoplastic polymer without compromising fluidity or mechanical properties of the final product is an eternal task of any compound manufacturer. This problem is especially of importance for manufacturers of HFFR cable compounds which are to combine high flame retardancy with smooth surface and nice elasticity. It is necessary to apply inorganic hydroxides (Al or Mg), particles of which are far from spherical shape and do not exactly promote elasticity. Moreover, any mineral filler contains some impurities, which cripple the ageing performance of the compound (the more filler there is – the stronger).

 

One way to solve described issues is to apply surface treated (or in other words surface coated) filler. Preliminary treating a mineral filler, especially of natural origin, with an organic agent allows to «deactivate» its surface – reduce moisture uptake, suppress interactions between impurities and polymer, improve filler-polymer compatibility and dispersion.

The most widespread and popular surface treatment agents are stearic acid, its derivatives and organo-functional silanes. Stearic acid provides good compatibility along with low cost. On the other hand, silanes provide additional features depending on the functionality, in example ability crosslink along with the polymer. In general, abilities and features of such agents are known, therefore the goal of present work is to investigate potential advantages of different combinations of components.

All agents were tested in a model formulation (Table 1), originally developed for synthetic ATH, replacing half of its quantity with natural magnesium hydroxide «EcoPiren 3,5» with appropriate surface coating.

Formulations Ref. Compound
Ingredient Trade name phr
EVA28 MFI=3 Escorene UL00328 70
mLLDPE d=0,918 MFI=3,5 Exceed 3518 20
LLDPE-g-MAH Fusabond E226 10
Silicon MB Silmaprocess AL1142A 3
Stabilizer Silmastab AE1527E 0.5
Fine precipitated ATH Apyral 40CD 160
Total 263.5

Table. 1 Model formulation of HFFR compound

On the first stage the effect of changing the level of Stearic treatment was evaluated (Table 2). Surface treatment with Stearic acid allows to improve fluidity and elasticity of the compound 10-15%. Increasing level of treatment after 1% does not further improve mechanical properties.

The effect of Stearic acid is definitely notable at 8-10% increased elongation compared to untreated grade, but it still doesn’t allow to reach Reference properties. Therefore, on the next step combinations of agents were evaluated:

  • «Dynasilan VTEO»
  • «Dynasilan 6498»
  • «Dynasilan GLYMO»
  • «Dynasilan AMEO»
  • «Pevalen»
  • «Esterex TM1111»
  • «TPSA»

Surface treatment was performed by preliminary homogenized mixtures of 1:1 ratio. The results are shown in Table 3.

All tested combinations showed higher Tensile Strength in comparison with Stearic acid. The mixture of TPSA and VTEO (FT40 and FT45) showed the best results. Its application increased the elongation at break 15-20% without the elongation at break 15-20% without significant loss of Tensile Strength.

Is it possible to obtain additional benefits using ternary mixtures? This was tested on the next step. Components were also premixed in ratio 1:1:1, immiscible combinations were skipped. The results are shown in Table 4.

No ternary mixture showed better results compared to binary one, though previous step best overall combination Pripol-VTEO-GLYMO performed roughly on the same level.

Thus it is possible to conclude that surface treatment provides a significant bonus to natural magnesium hydroxide performance and a possibility to introduce additional functionality. However, not every issue with natural mineral fillers can be solved by the surface treatment.

Formulations Ref. Cmpd FC 35 FT 35 FT 20 FC 34 FC 38
Base Ecopiren EP3,5 EP3,5 EP3,5 EP3,5 EP3,5
Coating None Stearic acid Stearic acid Stearic acid Stearic acid
Treatment (%wt) None 0.5 1.0 1.5 2.0
Properties Apyral EP3,5 EP3,5 EP3,5 EP3,5 EP3,5
Density at 23°C 1.497 1.496 1.489 1.481 1.485 1.500
MFI – 21,6kg @ 190°C 13 4 5 6 7 12
LOI 36 34 34 34 34 34
Tensile Strength 13 13 12 11 9 8
Elongation at break 180 135 140 146 139 144

Table. 2 Stearic acid treatment level effect on compound properties

Formulations Ref. Cmpd FT31 FT32 FT33 FT34 FT28 FT30 FT27 FT29 FT40 FT45
Treatment of Ecopiren (%wt) 1.8 1.8 1.8 1.8 1.8 1.8 1.8 1.8 1.8 1.2
Component 1 Pevalen Pevalen TM111 TM111 GLYMO AMEO Pripol Pripol TPSA TPSA
Component 2 VTEO 6498 VTEO 6498 VTEO VTEO GLYMO VTEO VTEO VTEO
Properties Apyral FT31 FT32 FT33 FT34 FT28 FT30 FT27 FT29 FT40 FT45
Density at 23°C 1.497 1.49 1.488 1.491 1.488 1.484 1.48 1.484 1.486 1.482 1.485
MFI – 21,6kg @ 190°C 13 4.1 6.2 5.2 7.8 6.1 6.3 8.1 7.6 5.6 8.2
Tensile Strength 13 12.2 11.5 12.4 11.7 12 11.7 11.8 12.2 11.5 12.5
Elongation at break 180 131 138 125 142 132 139 153 147 162 157

Table. 3 Binary mixtures treatment results

Formulations Ref. Cmpd FT23 FT24 FT25 FT26
Treatment of Ecopiren (%wt) 1.8 1.8 1.8 1.8
Component 1 Pripol Pripol Tego 6879 Pripol
Component 2 AMEO VTEO GLYMO VTEO
Component 3 Tego 6879 GLYMO Pripol GLYMO
Properties Apyral FT23 FT24 FT25 FT26
Density at 23°C 1.497 1.487 1.482 1.488 1.483
MFI – 21,6kg @ 190°C 13 6.9 5.8 6.2 3.4
Tensile Strength 13 11.3 11.2 10.9 11.2
Elongation at break 180 145 154 139 147

Table. 4 Ternary mixtures treatment results

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