Home Cosmetic Science Talk Formulating W/O Hair Cream - All Ears

  • W/O Hair Cream - All Ears

    Posted by Chemist79 on August 8, 2017 at 7:34 pm

    Hi All, I was wondering if anyone in the forum has had experience formulating water in oil creams, specifically for hair styling and could share any experience or suggest any improvements.  I realise this topic has been covered before but I can’t find any information that has helped me solve the issues I am facing.

    The benchmark is Brylcreem which I have completed 10 x freeze thaw cycles on and no separation is observed at all.

    My formulation is:-

    A - mineral oil 27%
    A - beeswax - 2.5%
    A - Lanolin Alcohol - 0.4%
    A - Glyceryl Stearate - 0.5%
    A - Stearic Acid - 0.4%
    A - Hydrogenated Rapeseed oil - 0.5%
    A - Hydrogenated Castor oil - 0.4%
    A - Phenoxyethanol - 0.4%
    A - Benzyl Alcohol - 0.4%
    B - DI water - q.s
    B - Potassium Sorbate - 0.2%
    B - calcium hydroxide - 0.3%
    C - Perfume - 0.25%
    C - Tocopherol - 0.2%
    C - Hydrolysed Wheat Protein

    I have tried a couple of methods both hot/ hot and hot/ cold

    Hot/ hot
    1. Heat both phases to 80C.
    2. Add B to A slowly with homogenisation 
    3. Once an emulsion is formed cool to 50C with stirring 
    4. Add C’s and homogenise 

    Hot/ cold 
    1. Heat phase A to 80C
    2. Mix phase B at ambient 
    3. Add phase B to phase A slowly with stirring 
    4. Add C’s homogenise

    I do not see a real difference in terms of viscosity,  appearance or stability using either method. The issue I have is that after 1 freeze thaw cycle I am seeing slight separation of the water phase (a few drops) and after 3 cycles significant separation of the water phase. So far I have not observed any stability issues at elevated temperatures.

    I have tried tweaks to the oil (23 to 30%) and beeswax levels (2 - 3%) and have also tried salts and glycol in the water phase but have not been successful in solving the freeze thaw stability issues. @Perry and @johnb have specifically mentioned the importance of the manufacturing process so I am wondering if my issues lie here? I.e mixing time and temperatures to fully saponify the beeswax.

    I have also tried including W/O emulsifiers like Glyceryl Oleate and Sorbitan Isostearate. Whilst this solves the issue it changes the performance of the product and the comb through is too long and doesn’t break quickly like a traditional hair cream should.

    Any advice or pointers would be greatly appreciated, many thanks in advance.

    zaidjeber replied 6 years, 6 months ago 6 Members · 14 Replies
  • 14 Replies
  • belassi

    August 8, 2017 at 10:21 pm

    You have no emulsifiers in there, to speak of.

  • bobzchemist

    August 8, 2017 at 10:48 pm

    Saponifying beeswax with calcium hydroxide is very likely your problem. As Belassi pointed out, it doesn’t produce an emulsifier. Try sodium or potassium hydroxide instead. 

    Alternatively, add the stearic acid that Brylcreem uses.

  • Chemist79

    August 9, 2017 at 6:12 am

    Thanks for the feedback I realise there are no traditional emulsifiers. The formulation is based on the saponification of beeswax with calcium hydroxide which is entirely possible. If I add emulsifiers then this changes the whole feel of the product and it doesn’t break down on the hair. I do have Stearic Acid in the formula,  Brylcreem uses Behenic Acid which I am struggling to source.

    The INCI for Brylcreem which I am trying to match is Aqua, Paraffinum Liquidum, Cera Alba, Hydrogenated Rapeseed Oil, Petrolatum, Glyceryl Stearate, Parfum, Limonene, Linalool, Citral, Geraniol, Benzyl Alcohol, Lanolin Alcohol, Calcium Hydroxide, Behenic Acid, Hydrogenated Castor Oil, Hydrolyzed Wheat Protein, Hydrolyzed Wheat Starch. 

    We have fully stability tested the benchmark and there are no stability issues on freeze thaw or at elevated temperatures.

    The benchmark contains no emulsifier and uses calcium hydroxide to saponify beeswax to stabilise the emulsion so I was wondering if it could be in the processing. 

    If anyone has any experience of this formulation type I would love to hear your thoughts, thanks.

  • bill_toge

    August 9, 2017 at 6:53 am

    if the ingredients list for Brylcreem is accurate, chances are it’s manufactured using a very high shear mixer (e.g. Ultra Turrax) or a colloid mill: your problem sounds very much like the droplets of the dispersed phase are not small enough to guarantee stability in relatively extreme conditions

    also, lanolin alcohol can help emulsify water into oil - it doesn’t work as a primary emulsifier, though

  • Chemist79

    August 9, 2017 at 8:22 am

    Thanks @Bill_Toge unfortunately we don’t have a colloid mill just a Silverson homogeniser. I will try increasing the Lanolin Alcohol,  I believe the Brylcreem INCI to be correct but think there is some clever labelling after the 1% threshold. I will try 0.99% Lanolin Alcohol. Do you know if Lanolin Alcohol performs better than just Anhydrous Lanolin? I have tried standard Lanolin at 1% but no major improvement on freeze thaw.

  • Ayman

    August 9, 2017 at 9:10 am

    I think you must change calcium hydroxide  with borax and you must add petroleum  jelly ac Brylcream formula

  • Chemist79

    August 9, 2017 at 9:13 am

    I have petroleum jelly in the formula, as borax and it’s salts have been listed by ECHA as substances of very high concern I would like to avoid there use

  • Ayman

    August 9, 2017 at 9:22 am

    Can you increase the percentage  of glyceryl  separate SE and stearic acid

  • Chemist79

    August 9, 2017 at 10:21 am

    I have tried Glyceryl Stearate and Glyceryl Stearate SE the Glyceryl Stearate works best. I have tried this in ranges of 0.4 to 1.5% no improvement on freeze thaw but the higher the concentration the waxes the rub in and the further away from the benchmark it becomes. I have tried Stearic Acid between 0.3% and 1.0% no improvement on freeze thaw and no real noticeable difference to the aesthetics. 

  • bill_toge

    August 9, 2017 at 1:18 pm

    the other critical factor is the temperature at which your emulsion is formed; it needs to be formed at as low a temperature as practically possible, or else it’ll destabilise as it cools

    try melting phase A, cooling it, finding the approximate temperature at which it sets, then forming your emulsion 5-10°C above that temperature

  • Chemist79

    August 9, 2017 at 1:53 pm

    Thanks @Bill_Toge I will give this a try, much appreciated 

  • bobzchemist

    August 9, 2017 at 8:33 pm

    The Beeswax/Calcium Hydroxide reaction will probably take either a high temperature or a long time to proceed to completion. You might need to try running that reaction before you make your batch, although I still think you’d find out valuable information if you tested a range of neutralizing agents.

    If you’re already using the Silverson with the smallest possible screen, sometimes extra mixing time can make up for the use of a lower shear mixer.

  • Chemist79

    August 9, 2017 at 8:44 pm

    Thanks @Bobzchemist I have tried TEA, AMP & NaOH all with no success with the exception of Borax nothing works as well Calcium Hydroxide so far. I have tried 80C and I don’t think a higher temperature is feasible for full production given our mixing vessel capability. However I think @Bill_Toge may be onto something regarding forming the emulsion at the lowest temperature possible.

  • zaidjeber

    August 14, 2017 at 1:50 am

    @Chemist79 try adding some xanthan gum, it might work! & lets see what others think about this? 

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