Benz3ne
Forum Replies Created
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What ‘powder’ are you referring to? Should it have fully dissolved and if not, why not?
All we currently know is that it is an oil with powder, that is then used to make an oil/water mixture and that you’re assuming that it is not correctly emulsified, but that the powder not being dissolved is possibly the issue.
I’m afraid we’ll need a little more information to help. -
Belassi said:I did not continue with this experiment so I can’t comment further.
It’s a shame you’re not commenting on some of the points raised, in case someone wants to satisfy their curiosity and try and replicate/resolve the issues you experienced.
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crillz said:Thanks Benz3ne, thought as such, good to get clarification.
Very welcome.
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minniemouse said:That’s what I’ve been doing, but i’m still not able to ground it fine enough. But thank you for taking the time to respond back.
Very welcome. I’d be tempted to find a supplier who would give you a fine enough powder to incorporate without issue.
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Kunal said:@Benz3ne.. Hey.
So best way to maintain the viscosity is to keep the solution in air tight container. Right?
I also found that shampoo which I have kept in the small bottle with screw cap pack in the month of Feb (before lockdown) almost lost 20% volume after lockdown (July).
So the best way to minimize the water loss might be to package it sealed.
Is that right?Hey my friend. Yes, absolutely. Although, I’m surprised that it lost 20% over 5 months in a small bottle with a lid on, regardless of it not being air/water-tight.
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Had fun trialling this one with a spare 5 minutes available.
Tried as hot process as it was quicker than leaving things cool down and allowed me to add the stearic acid as liquid rather than trying to incorporate a semi-solid stearic acid/coconut oil/sunflower oil (as didn’t have palm to hand, adjusted for sap values).
Pretty well as two phases, didn’t get around to preservative or fragrance, added with mixing with an immersion blender.
Nearly instantly (as to be expected with Stearic Acid saponification) formed lumps of reasonably solid masses, so not thoroughly homogenous. pH was holding high around 11-13 for the accessible bits. As if there wasn’t quite enough water added, or that it crashed the potassium stearate out quicker than anything else could happen (more likely).
Would be interested to hear whether you did this as cold process, which I’m assuming you did.
Funnily, adding more water and blending the mixture allowed me to fetch the pH down closer to 9-10, though was a bit messy. The resulting liquid foamed quite nicely and had a reasonable amount of slip to it, so I’d like to think that the original mixture would’ve been nice until it had separated.
I did notice that the outer interface of the solid masses was a little ‘bouncy’ so assume that it was more gel than ‘cream’ in consistency. Fun little trial, unfortunately with no answers to your conundrum. -
ketchito said:@Kunal A way around is increasing the relative content of the anionic (eg., 4:1:0.5). Also, these type of products when left in an open container, tend to gradually lose water, that’s why you see it becoming a gel over time.
This is what I’ve gone for in my trials and that’s working nicely and repeatably.
Agreed with your point about water loss and subsequent gelling - @Kunal you can see this first hand. Make a batch of your shampoo and squirt a little into a weighing boat and leave it out in the open. Give it a stir the next day and it’ll be thicker. A stir the following day and thicker again. You could go one more than this and weigh at intervals to see how much water loss has how much of an impact. -
There’s no harm in boiling your water and leaving it cool to ‘sterilise’ it, though your preservative should do a decent job. Good lab hygiene and cleaning practices help here. Rinse things out with isopropanol before using them will help reduce contamination too.
75-80°C will kill some things but not all things, so you’re doing half a job by bringing it up to that temperature alone. -
What is limiting your shelf life?
If it is oxidising, include an antioxidant like Vit E (tocopherol/tocopheryl acetate) or if it’s spoiling due to bacteria, include a broad spectrum preservative. -
Very interesting. The only possibility I can really think of is that there were more ‘active’ ingredients added prior to/during saponification. I’d have been inclined to saponify the stearic acid, coconut oil, palm oil separately to make your shaving cream ‘base’, with your solution of KOH and NaOH and add the TEA, glycerine, fragrance, polyquat and preservatives thereafter (perhaps with some in solution).
I’d be surprised if you had got this aspect wrong, given your repertoire.
I might actually give this a go a little later and see if any separation does occur.
The only other thing that might be worth noting is rates of saponification. IIRC stearic acid reacts very readily to form sodium/potassium stearate, so that will oftentimes ‘mop up’ a reasonable amount of the NaOH/KOH (probably useless info here). Otherwise, it’s reasonably KOH-heavy, so would be a little looser than if more NaOH was subbed in. -
Majman said:A body lotion @Benz3ne and the ph was too acidic and to reduce it, I divided the cream into two, added caustic soda in one and lye in the other and ended up foaming and overflowing out
I’m curious as to why the pH was so low also. If adding sodium hydroxide (as a solution rather than pellets, right?) caused foaming/overflowing then something is reacting to create gas… doesn’t sound right to me.
Sodium hydroxide = lye = caustic soda, so we’ll need clarification on this point as to what exactly you’ve added, or differed between the two trials you’ve conducted.
Try TEA as @Pharma has suggested above.
Read up on pH as well, it’ll give you a good idea of which direction to go and how to do that. Also be worth looking into soap making, as if you’ve free oils in your mixture (body lotion) then you have a potential to saponify them by adding caustic soda/lye/sodium hydroxide/potassium hydroxide/potash creating soap. -
Triethanolamine, I have found, struggles a little with hydroalcoholic gels towards 70%, so 73% will likely be a little unpredictable.
I’ve found for 0.3% carbomer 940 that approximately 0.27% aminomethyl propanol does a good job of bringing the pH down to around 6-7.
This .pdf states ratios but doesn’t touch on maximum ethanol concentrations (page 2, table 1) https://www.lubrizol.com/-/media/Lubrizol/Life-Sciences/Documents/Literature/Bulletin-05—Neutralization-Procedures.pdfBe mindful that you’re asking two separate questions. You’ve asked (a) how much TEA is required for pH6-7 and (b) please confirm that adding more TEA will increase viscosity.
TEA isn’t the thickener, the carbomer is as I’m sure you already know.Neutralising the carbomer is what increases the viscosity, so if you want greater viscosity, you need more carbomer and to then neutralise that. 940 imparts a large viscosity at small concentrations, so note that small changes can make a large difference.Hope you are safe and well also.
Edit: 0.5g per L of product is around 0.0625% TEA (given 70% ethanol solns are approx 0.8g/mL). That won’t be enough to neutralise the carbomer completely. Try focusing on the w/w% of the TEA you’re adding. There’s usually a reasonably wide ‘shelf’ of neutralisation so pH will only jump up after the carbomer is neutralised.
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Visiting this old thread and not sure whether you’ve resolved your issue.
Depending on the soap used you might get some thickening in hydroalcoholic (including ethoxylated alcohols) solutions under heating. I know that to be true for sodium stearate so there’s no reason it might not be true for other soaps. -
Where are you based? Your national biocides regulations typically dictate how to label/test products or what the test criteria might be.
This is muddied a little in the EU currently as ethanol is an ‘under approval’ substance so there’s a general application of the regulations which is then amended by the country in which you want to sell it - unfortunately these amendments can vary massively. -
What is confusing you? Try them out - you should get a good amount of foam from each of them if you have a high enough concentration of active matter.
CDEA is a personal choice - it shifts the salt curve so you typically require less salt than without it to thicken the mixture.
The amount of foam you produce might also depend on your other ingredients, glycerine typically kills foam and viscosity (you’ll see that mentioned a lot here) so try removing that (if you’re using it) and see what effect it has.
As for economic pricing, that’ll all depend on where you’re based and how much you can buy x amount for. It might be more expensive for me to buy SLES than for you, so I’d be less inclined to buy SLES.
For what it’s worth, my mixture is 4:1 SLES:CAPB with a small amount of CDEA added. I’d started with around 5% glycerine but that gave hugely inconsistent results so dropped to 2% (in theory could drop further) and added 0.1% Polyquat-7 for slip and that’s working nicely for me. For small quantities (50mL flip caps) I’m sticking around 0.9% of a 10% NaCl solution for thickening, and for larger amounts in pumps I’m doubling that. Working consistently despite trying with a variety of essential oils for fragrance.In short: Have a play around and see what you come up with, and don’t be afraid to compare costs or look at bulk prices at this stage.
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How does the filling nozzle operate? If it’s ‘dropping’ the load of hand soap from height, at speed, then it’s more of an engineering issue than a formulation issue.
Belassi is undeniably correct about 18% being particularly high. 12% is what I’m currently working on at the moment and that’s nice.
I’ll agree with Belassi also on leaving it settle after batch production, any air bubbles in the bulk mixture will only exacerbate the dispensing issues. -
You should be able to purchase your inorganic pigments as small enough particle sizes for incorporating into your mixture.
What I have found, if ever I need to mix inorganic pigments into bases (granted, they’re solid suspensions that result and not liquid) is to mix your pigment into a small portion of the base you’re aiming to use and then incorporate that into the rest of the base.
That said, they should simply mix with reasonable ease. Typically nail polishes have a ‘mix well before use’ type of clause anyway so some settling of pigment
isn’t unheard of. -
filiz said:@ozgirl @mhart123 When I talked to my raw material supplier, she said that the magnetic stirrer is not sufficient for mixing.
She said different thickeners wouldn’t work either without high speed mixing.
Do you think the problem could be entirely due to this??Possibly, but you won’t know first-hand until you try it.
Give it a go with a cheap hand blender/stick blender and see whether it still exhibits the same issues. It might end up foamy for a day so leave it sit and see what results. -
How are you mixing this?
I can’t see any reason why this would be separating unless you had salts in the water that don’t get on with your pearlising or gelling agent.
Is your pearliser a cold-process or hot-process, too? -
Pharma said:What exactly are you making?
My first thoughts too.
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10% is on the milder side of normal for hand washes. pH looks fine to me too. The Benzalkonium chloride shouldn’t have much of an impact on skin dryness if it’s used in small percentages.
Re-looking over your formulation, I’ve seen mention of glucosides being reasonably cleansing of lipids/fats/oils, so to add refatting agents. I’d say that’s a good place to start and see how you get on with that. -
You’ll probably want a refatting agent or conditioning agent.
The two go-to’s are glyceryl oleate or polyquaternium-7. I’m sure someone else might give some suggestions.
What % actives do you have and what’s your resulting pH? -
@Oladoo you need to include more information before people can help you. What type of oil? Fragrance oils and/or aromachemicals? Or do you want emollients? Why 10% and 70% in particular? Are you trying to amend a current formulation you have, in which case what ingredients are you currently using?
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Karen said:Percentage symbiomuls GC is 5%
I emulsify with a dynamic MX100
The longer and more high shear seems to make it separate more and when I tried by just stirring at the end after emulsification it brings it back together - if that makes sense.Put the other %s you’ve used and that’ll help determine whether you’ve enough emulsifying agent.
I would assume that you need a high shear initially until a grain-free emulsion is formed and continual stirring thereafter until cool.
The separation might be because you have something that has not incorporated into the emulsion, or that your emulsion isn’t stable as a result of not enough (or wrong type) or emulsifying agent. -
To OP - I’d also second dropping the % of glycerine. I’ve noted from my own trials that glycerine inclusion does inhibit foam production and lowers viscosity (typically).
Have you compared the surfactant blend in the standard market product to yours? Typically mixtures are SLES/CAPB only or sometimes include a little CDEA, so maybe just try those two and scale-up actives of those two to 12%, thicken with salt and see how the lather differs.
You might actually have a preferable lather, but bubbles might be smaller. Or that you require a little more water to lather the product.
I’ve read into handwashes/bodywashes being up to around 20% actives, so you might want to experiment with concentration of actives, up from the ~13% you currently have.
For records, I found that ~12% actives across an approximately 6:2:1 ratio (SLES:CAPB:CDEA) has lathered just fine, comparably to other marketed hand washes.