[luiscuevasii]

@Pharma thanks for your reply, im a Chemical engineer, so my knowledge of small scale procedure and lab is almost None, i made the experiment in a bigger batch, and eureka, there was a lot of glycerin after salting, separation and evaporation.  

Right now im looking to clarify the remaining glycerin, it has a dark brown color, i have tryed with reverse-osmosis and mixing with activated charcoal at 90°celcius and the brown color remains

[luiscuevasii]

@Pharma  yes, indeed im salting out the soap, but i belive that the glycerol separates from the tri-gliceride molecule when neutralization ocours and salting out is used for taking the glycerol and all the non-soap sustances with water.  Im making right now a 50liters evaporation, so far i have made only laboratory batchs,  i must have arround 5kg of glycerol acoording to the texts books. 

[luiscuevasii]

@Pharma my first guess was that i didnt had glycerol and something went wrong with the saponification, but saponification is a  very standard reaction, after is complete i use salt to precipitate the glycerine, water, impurities, naoh and salt.  If the saponification went wrong i must have two results:

#1 a soap with a lot of unreacted oils, ór
#2 a soap with excess naoh plus salt

The batch where i draw the Glycerol-salt-naoh-impurities, was a 5ton batch, the soap obtained was excellent, so i can assume that i must have Glycerol on the spent lye

—-

I did evaporation two times, but the result was the same, only brown salt was left

[luiscuevasii]

@Pharma thanks for your answer,  it’s kind of difficult to have less water in the initial product, my initial goal is to separate de glycerol, excess naoh and salt from soap, and having excess water is very helpful.

By the other hand, I have made experiment evaporating the water at atmospheric pressure 110celcius, and I’m not having glycerol in the residue only brown salt, so I was guessing that must be and azeotrope.

Almost all the literature I have read so far uses vacuum distillation  , I’m capable of using -600 to -720 vacuum in laboratory and in big equipments, but I did trials with the same results as the atmospheric distillation. For example I made one trial at -700mmhg 120celcius, and I was left with only salt at the end, and other trial -700mmhg 200 Celsius with the same result.

I thinkt that using several condensers in series could work like a fractional distillation, but any input would be helpful, working with out the proper guidance is troublesoem

[luiscuevasii]

Yes, you might, i mean, i have a 25hp selfmade inline homogenizer that has no trouble sucking 70% sles, some times it became crystal and i have to pour water with a hose, and some time it get stuck but playing closing/opening the valves the problem solves.   its not my preferred proccedure, but i have made it a lot.  

Right know we use double diaphagram pump for sles, i make 6.000liters batch that requieres two and a half drums of sles, its faster ussing a pump and requieres no-cleaning after, i just put the pump recirculating and it self-clean.

[luiscuevasii]

Pharma said:

I’m sorry, they all won’t work. These are organic acids and they are simply not acidic enough to activate other carboxylic acids or esters.

Use calcium oxide or potassium carbonate to make biodiesel and use that to produce whatever you want . Although it’s two reaction steps, you still will be faster, a lot faster than with the acid route.

What about working with 20% concentration HCl, I mean, I know I can try and see, but I know you have a wonderful knowledge and any input would be appreciated. HCl is under “strict” control but I could get a diluted solution in small quantity

[luiscuevasii]

Pharma said:

Citric won’t work at all or at least not sufficiently enough.

Phosphoric acid has a bunch of drawbacks:

- It is a rather weak mineral acid if compared for example with HCl or…

I want to thanks for all your help, my country right know is synonym to “that hard”, so everything here its a little complicated but no imposible. I mean, beginning that every raw material to be imported must be Profitable for importers, right now we are just barely achieving the basic needs, so everything that isnt food its bassically not available. Thats why almost in all my post im trying to make products from basic and raw materials, wich is very frustaiting, i mean, im trying to reproduce products that are arround 30years all or more.   

But im very optimist, and having no competitors has its advantages. 

Im a engenieer, so im not familiarized with deep knowloedge of catalysts, i will give you the acids availables and if you could keep help me i will appreciate:

acetic, oxalic, formic, propionic, salicylic, fumaric, tartaric, malic, lactic.

[luiscuevasii]

@Pharma I’m so sorry, Im planning to use citric or phosphoric acid, I misspelled and confused the resction because I was thinking in biodiesel.

For olivem I have those acids available

[luiscuevasii]

Microformulation said:

No offense, but in my opinion most Formulators move away from Olivem and others such as they grow in skill and familiarity with better and newer emulsifiers. You rarely see either in mainstream commercial products.

It’s not offensive at all, I’m aware, I just want to have a product that could make “natural” consumers well.  I know that there are plenty of new and better emulsifiers, but in my country basically we can only emulsify with Sles, peg100 stearate, GMS, tweens, and cellulose polymers like Hemc.

There aren’t options, we are under a USA sanctions and economy here isn’t going well, so importing emulsifiers is not a priority.

[luiscuevasii]

Pharma said:

If you want to perform transesterification, use base catalysis and go the detour via methyl ester .

Acid catalysis works but takes time and/or high temperatures. Also, polyunsaturated fatty acids don’t do well with sulfuric acid (@luiscuevasii it was you who can’t get that anyway, right?). 

Thanks for your input, yes, I’m the one that can’t work with sulfuric, nitric and clorhídrico. 

I was planning using Naoh and methyl ester route, I had made biodiesel before, and glycerin for example just go down and separate.  

[luiscuevasii]

@Microformulation Thanks you very much, i just wondering if someone did something like olivem, it looked like a simple procedure. im familiarized with esterifications and i have lab and medium scale equipments for sterification, but working with only oleic/stearic acid comming from olive oil and pairing an alcohol in acid catalyst its more difficult than simple transterification.

I already have other surfactants, but i want to offer something more “natural”, and there are a lot of olivem fans out there.  

I think that i have the equipments, but i will appreciate any input.

[luiscuevasii]

It seems that white sugar doesn’t have nutrients for the yeast to grow efficiently, and the yield goes from 15-25% in both cases. I will appreciate any input 

[luiscuevasii]

@Pharma thanks you again for your help, I was looking for making a more comercial raw material.

[luiscuevasii]

ngarayeva001 said:

HCO might be useful as a thickener in anhydrous products such as lipbalms, and interestingly enough is used as a physical exfoliant (which is added to cool down phase as a powder).

Thanks you very much, we used it for thickening deodorant bar, but the project stopped

[luiscuevasii]

I’m not an specialist, but I was very surprised when I found that stearic acid in powder form, it is not only stearic, in fact there is a lot of Oleic. It seams that isn’t easy to split both products. 

I have used flakes and powder, and got better results with the powder in terms of hardening the soap. By the way, are you using SCS for your sunset bars?.

[luiscuevasii]

@Pharma thanks you very much, your input its always very valuable, i think i will drop the project with the HCO, i dont know what else i can do with it.

Right know im ussing it in a cream subtituting a little of stearic acid for it, but i think it would take arround 4 years to use all the hco i have.

talking about labsa you are right, it could make an emulsion with the oil, i asked because i saw it in a pattent and im looking for a catalizer that could be bought easy in my country.

[luiscuevasii]

I mean, castor oil is composed 80-90 ricinoleic acid, I think simple sterefication would be possible.

By the way, in other post I asked about acid catalizers for sterefication, I can’t buy sulfuric or nitric, you recommended phosphoric, but what about Alkyl bencene sulfonico acid instead? @Pharma

[luiscuevasii]

@Pharma what do you think about making an sterefication between castor oil and peg400, under acid? .

I think that’s what they do with stearic acid and peg100, a sterefication that leaves peg100-stearate. But I dont know if I can use the HCO as a organic acid.

[luiscuevasii]

Thanks @Pharma for your input, I do have a small lab, but I’m not a lab especialist, in fact I’m an engineer so most of my lab knowledge is empirical. I also have big reactors with jackets for steam and water, and reflux capability.

I can’t work with ethklene oxide because its cancirogemic and I need special permissions to work with. But there’s a small factory that makes some peg products like peg100-stearate that works with stearic acid and peg products, with out etoxilating directly

[luiscuevasii]

Cafe33 said:

Is this a singular component for you to suggest purification by vacuum distillation?

You will have to think of a drying step after steam distillation, one that does not effect the oil. Maybe you can find a book about the subject.

Thanks you for your answer, I’m using sodium sulfate after distillation. 

[luiscuevasii]

Usa

[luiscuevasii]

@Pattsi

Thanks you for your input, are you an user of Eucalyptus oil?, i mean, i want to know to whom or what kind of factory i can offer the Oil.

[luiscuevasii]

Coconut oil has almost the same lauric acid concentration

[luiscuevasii]

Ussually we use salt (brine) in order to saturate the soap with electrolytes and precipitate all the “no-salt” compounds of the soap (sodium salt of fatty acid), the brine separates mainly the glycerin and impurities of the soap and brings they to the bottom of the reactor-tank.  this procedure is only made in old factories like mine that use crude vegetable-animal fats as raw material for soap. Some (trazes) of the salt could remain on the soap.

newer factories splits this Fats (triglicerides) with high pressure steam (30-50bar) and remove the glycerin before the saponification reaction, they do not need the salt.

[luiscuevasii]

Greetings, well, im not longer making deodorant with potassium alum, due to the poor effectiveness of alum as antiperspirant. by the other hand, the pH was not a issue, in fact the pH was very difficult to raise, beacuse ussing naoh or triethanolamine would convert the potassium alum to NaAlO2, wich is insoluble in water.