Making a White Carbol / Phenyl

Hi.. my name is ryan. i am trying to make a blend of pine and citronella oil in water emulsion.
the formulation i use is 10% of emulsifier (abt 6mL) nonylphenol-9 (HLB-14), Citronella oil 35mL (HLB 12.6), Pine oIl 25mL (HLB 16) and water.

the process, 
1. I mix both oil, and blend it for few seconds using normal hand blender, and then pour in the 10% (6mL) emulsifier and blend it again for few seconds

2. i started pouring in water which already pre-mixed with CMC(Thickener) slowly until i get a thick white emulsion, 

3. I poured the whole thing into a juice blender so that i can get higher RPM, and keep adding in water up to 500mL, and transfer to a liter Jar where i added another 500mL of water.

4. the whole solution appears milky white and thick. and i thought i managed to get a perfect emulsion

5. the following day, to my surprise, Creaming happen or white fluid float on top while the rest on the bottom of it I believed is water.  This means my emulsion is not stable.

I need help on whats wrong and what can be done to make it right ! PLEASE HELP

Comments

  • Did u do any oil heating? 
  • BelassiBelassi Member, PCF student
    Apart from anything else, I don't think you had high enough shear at any point in the process. I guess you discovered that 10% of that emulsifier is not enough.
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  • DASDAS Member
    Your product turns white because you are not emulsifying properly and you are adding a lot of water to an oil. You can't make an emulsion with that 10%, that's about 0,5%, it should be 10% of the total formula. 
    The oils don't have HLB because well... are oils, they don't mix with water. The HLB system is for surfactants.
    And the CMC is pH sensitive, you would have to adjust it.
    And it is a lot of blending that you don't need, you will get a best result and less foam and air with a spoon.

    What I don't understand is what kind of product are you trying to make, even if you stabilize it you will end up with a smelly gel. 

  • Thanks for the Reply.

    @fkay, i dint do oil heating as to save time in making the product, do i need to heat the oil ? 

    @DAS , thanks for your input. so if in this particular case, i want to make a Litre product, i will have to have 100mL of surfactant and same amount of oil which is 35mL Citron Oil and 25mL of Pine ? isnt it too much of a surfactant to use ? 

    I have tried using a wooden spoon during the blending, and i found it seperates even faster as i supposed the whole thing doesnt blend properly.


    I am trying to make a floor cleaning formula which has a disinfectant affect and also a bug repellent property in it. 

  • DASDAS Member
    I see. In that case the more surfactant you have the better, a floor cleaner with little surfactant won't be cleaning much. So match it or double it. 
    And the oils are not disinfectant at all, at least in that percentage. And legally you would have to have in your formula an approved material in a minimum percentage to be able to call it disinfectant. Benzalkonium chloride is the most commonly used.
  • @DAS thanks for the kind reply. I havent tried the doubled amount of surfactant, but i found 4% of total formula is sufficient to make it white and quite viscous. 

    do you think by adding more surfactant it will cause even whiter and more viscous ? i am actually want to make a concentrate formula. 
  • DASDAS Member
    It will give more stability, even if you product seems stable I don't think it will stay that way through time. 
  • @DAS hi das. i found that adding too much of the surfactant solved the creaming problem, but another problem occur, it seems that the mixture started to break down, it doesnt suspend and it doesnt float. its hard for me to describe here. anyway, can you give me hint . let say i want to make a 4L mixture and it contains 1.5% oil, 1% surfactant, 2.5% Thickening Agent (CMC), and the rest is water.

    I started by mixing the Oil and Surfactant and do a gentle stir with a wooden spatula, and then add slowly the thickening agent so that i get a nice thick milky lotion like solution, and then i poured in the water slowly. 

    at first it was all nice, adding so much water the solution became watery and not as milky white as i want. please do give me some hint on how to have a milky white solution :'( been wasting alot of expensive oils and surfactant and yet to get the result that i want.

    Below always happened, been trying to make a perfect one but failed i think about 50 samples with different composition.
  • If it gets white is because you are doing something wrong. The NP and the CMC are both transparent in final product. It gets white because you are having a o/w fist fight or because the CMC is out of pH. Or maybe both. 

    As I suggested match the NP or double it (1,5-3%). And for the CMC the pH should be 7-9. You should get a nice transparent thick product. If you want to make it white you should add an opacifier like styrene/butadiene, or maybe it's gelly enough to add a microdispersion of titanium dioxide.
  • @DAS well, i wanted it to be natural white look on the product. i have tried TItanium dioxide powder, and it wont mix or dispersed completely in water. over time it will settle down at the bottom of a jar. 

    I havent tried styrene/butadiene as i try to make a product with least chemicals involved . so i want to look as natural white as possible, that is why i am always having problem with the emulsion. is there any natural way to make the product white ? 
  • If you use the powder it's impossible. It's not water soluble. But you are using CMC. If you make a stable formula it might work.

    Considering you are using NP I don't see the problem over a little bit of styrene butadiene. There are non-ionic of white appearance, but I can't think of any for the use you need.
  • @DAS the styrene, isnt it oil based ? will it easily dissolved in water? 

    i tried Titanium dioxide before with the help of CMC (not stable yet). i can see the TiO2 settled at the bottom.. =.=
  • No, it's a latex. Works great in water and it's cheaper and easier to use.
  • @DAS lets say i get a stable milky emulsion in a 2L jar. inside i have 1% of oil and 0.25% surfactant.. if i want to make a 90L solution. can i multiply the amount of oil and surfactant by 45 and it still give me the same end result?
  • You will get the same result, which is an unstable emulsion.
  • @DAS is it that hard to get a stable emulsion ? 
  • ozgirlozgirl Member, PCF student
    It shouldn't be too hard to get a stable emulsion but you will have to do some trials.

    You will probably have better luck creating a stable product using a combination of emulsifiers/surfactants (a blend of low HLB and High HLB) or even adding some ionic sufactants.

    For the record Nonylphenol ethoxylate-9 is not a natural product.

    Have you searched for formulas for this type of product?

    http://www.pinoychem.com/2013/05/pine-oil-as-disinfectant.html

    http://www.pinoychem.com/2010/11/blooming-pine-oil-emulsion-concentrate.html

    I would also recommend working in grams and not volumes.

  • Chemist77Chemist77 Member, PCF student
    Surface cleaners are not really viscous even if you want to dilute it. Why don’t you use Benzalkonium chloride as someone suggested @2-3% and you can still dilute the final formula upto 20 times. Use a non ionic surfactant like an APG at around 0.5% and another non ionic like Berol 260 @1-2%, it will give you a milky emulsion. Use a defoamer @0.005% level to minimize the foam while cleaning. 

  • @ozgirl
    "You will probably have better luck creating a stable product using a combination of emulsifiers/surfactants (a blend of low HLB and High HLB) or even adding some ionic sufactants.
    can you recommend what kind of ionic surfactants that i can use?

    For the record Nonylphenol ethoxylate-9 is not a natural product. "
    i am aware of this. but I have searched and read some in the forum that np-9 should be fine. maybe do you have anyother surfactant that will give me a stable emulsion and its natural ? 


    @Chemist77 it seems you mentioned alot chemicals, I am trying to make as less chemicals as possible. thank you, i will definitely consider those.
  • Chemist77Chemist77 Member, PCF student
    It seems 3-4 ingredients are lot for you, good luck then!!!
  • chemicalmattchemicalmatt Member, Professional Chemist
    ryanou, this is simpler than you may suppose. You only need to add a hydrotrope as co-surfactant here, as nonoxynol-9 is a not exactly hydrophyllic, despite any HLB value attached.  I suggest disodium cocoamphodiproprionate, a useful amphoteric hydrotrope (Solvay, Ele' for sources). A little dab will do 'ya. Also, CMC doesn't have any yield value to suspend whatever is to be suspended. I'd drop it.
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