Should I dilute sulfonic acid before neutralizing it with Sodium hydroxide ?

Gunther

Member

January 23, 2019 at 2:54 pm

agagag said:

I’ve got another question. I made neutralisation and after night I get product with pH 8. But my sample delaminate…On the top my pH is 8, and on the bottom pH is 12. Should I change the quantity of NaOH…?

What’s LABSA concentration?
Some low grade LABSA have trouble getting past 15%.

Also, you can try neutralizing it with Sodium carbonate (Soda ash) instead of NaOH to see if it works.

Chemist77

Member

January 23, 2019 at 3:28 pm

I add my alkali first to water, then LABSA. Can always adjust pH slowly at the end.

agagag

Member

January 23, 2019 at 3:45 pm

My LABSA is 95% and I dilute it into 30%. Than I am adding 30% NaOH and I have delaminate salt. Tomorrow I will mix it as @Chemist77 wrote

Gunther

Member

January 23, 2019 at 4:23 pm

Is that 30% total LABSA in your finished formulation?
If so, this is too high a concentration.

Also, 30% LABSA doesn’t need 30% total NaOH to neutralize
search for LABSA and NaOH molecular weights, to get the relative proportions to each other.

agagag

Member

January 23, 2019 at 7:04 pm

Thank you @Gunther. Yes, now I am searching for the best proportion to get neutralized product. I am also checking how long my neutralitzaion will take.

khoikhoa

Member

January 24, 2019 at 4:01 am

you should dilute LABSA before neutralize by NaOH (30%), for get pH 8 , use NaOH then adjust by TEA

imasoat

Member

January 24, 2019 at 9:42 am

Thank you guys for educating us.

What percentage of NaOH & LABSA is
required too get a clear & transparent mixture with relaive thickness/viscosity. What percentage of
water should l use to dissolve the NaOH.

Do l need to dilute the
LABSA, if Yes, what water percentage is required and what is sequence of
mixing the ingredients.

Chemist77

Member

January 24, 2019 at 1:14 pm

@imasoat anything upto 20% should keep you good plus if you have other surfactants. I use around 12% plus few other surfactants and the results are pretty good.

agagag

Member

January 24, 2019 at 2:51 pm

…I think my LABSA is not so pure as I thought…@Chemist77 do you know how long did you mix LABSA with NaOH to get pH8?

Chemist77

Member

January 24, 2019 at 5:17 pm

Mixing period will not decide the pH, your acid to base ratio will.

Aziz

Member

January 25, 2019 at 4:27 am

shaujaat said:

aaaaaa There is no problem with your material….. It happened to me as well with the same material I uses, what I think what happened was I didnt gave time to each liquid to dissolve completely and poured whole of it at once. It is better for your to divide the water that you are going to use in the process in to two and dilute the sulfuic in the water and then pour slowly the NAOH to neutralize it. don’t mix it with other materials until it cools down, that’s my experience

Perhaps this is one of the most valuable comments of this thread . I faced same problem at first and then over come it by following the Rule ,
‘ Never put your second ingredients until your first one is completely dissolved ‘ .
Dissolve NaOH in adequate of water , then pour LABSA slowly with stirring over a 15 to 20 minutes of time and continue stirring until completely dissolve and get a transparent solution .
Hope you will overcome this problem .

Gunther

Member

January 25, 2019 at 5:15 pm

For the same amount of LABSA (preferably <20% in the final formulation)
try neutralizing it with both NaOH and Sodium carbonate (in proper proportions to each other, so Google LABSA, NaOH and Sodium carbonate molecular weights)

I got a feeling that the strongly alkaline NaOH degrades LABSA, unlike the milder carbonate.

Gunther

Member

July 9, 2019 at 6:35 pm

This study states neutralized LABSA cloud points as:

https://ejchem.journals.ekb.eg/article_7631_aed50d75c833b783095ca669b368d51a.pdf

This might explain why I had trouble getting clear formulations beyond 15% neutralized LABSA.
While I was able to get some clear 15-20% sulfonate formulations at room temperature, I’ll see if they cloud at low temps.

Also, the study shows that cloud point is highly dependent on salt content.

RedPill

Member

August 2, 2019 at 11:12 am

@Gunther Did you overcome this isse? I am also facing the same problem.
Mixed 200ml LABSA with 200 ml water.
Ph balanced approx 7 with 50% caustic solution.
After 8 hours normally we can expect a transparent liquid. But in this case the solution is solid thick white paste.

Gunther

Member

August 2, 2019 at 11:41 pm

RedPill said:

@Gunther Did you overcome this isse? I am also facing the same problem.
Mixed 200ml LABSA with 200 ml water.
Ph balanced approx 7 with 50% caustic solution.
After 8 hours normally we can expect a transparent liquid. But in this case the solution is solid thick white paste.

Some things that help avoiding/managing this:
1 Predilute LABSA with water. Add a water volume/weight at least equal, preferably twice LABSA weight.

2 Predilute solid NaOH in water

3 Always add NaOH solution slowly to the LABSA solution, and never the other way around. It looks like an alkaline pH causes the problem, while an acidic one lessens or avoids it.

4 Don’t add any further NaOH beyond pH 8.

5 You can try slowly neutralizing it with a 20% Sodium carbonate solution. While it generates a lot of bubbles and you must wait for them to dissipate, it’s harder to overshoot pH into the alkaline range with Na2CO3 than with NaOH.

6 Some manufacturers LABSA cloud right when pH gets past 7, despite using Sodium carbonate instead of NaOH. Switching LABSA suppliers is a must then.

7 Don’t add any salt to it, it just rises cloud point.
If you need a thicker product, add more neutralized LABSA, SLES, CAPB or both.

RedPill

Member

August 6, 2019 at 4:40 am

@Gunther Thank you for your very detailed procedures.

Aziz

Member

August 6, 2019 at 11:47 am

Gunther said:

For the same amount of LABSA (preferably <20% in the final formulation)
try neutralizing it with both NaOH and Sodium carbonate (in proper proportions to each other, so Google LABSA, NaOH and Sodium carbonate molecular weights)

I got a feeling that the strongly alkaline NaOH degrades LABSA, unlike the milder carbonate.

My dish wash is transparent, thick and stable at 4°C but foam is not so well.
How to achieve sufficient foam in final product ?
Which of ingredients degrade foam ?

Gunther

Member

August 7, 2019 at 1:40 am

Aziz said:

Gunther said:

For the same amount of LABSA (preferably <20% in the final formulation)
try neutralizing it with both NaOH and Sodium carbonate (in proper proportions to each other, so Google LABSA, NaOH and Sodium carbonate molecular weights)

I got a feeling that the strongly alkaline NaOH degrades LABSA, unlike the milder carbonate.

My dish wash is transparent, thick and stable at 4°C but foam is not so well.
How to achieve sufficient foam in final product ?
Which of ingredients degrade foam ?

What’s the formula like?

Aziz

Member

August 7, 2019 at 3:25 am

@Gunther

LABSA 8%
NaOH To pH 8.5
EDTA .2%
Na citrate .5%
SLES 4%
SLS 1%
TSP 1%
CDEA 3%
CAPB ( 30%) 4.5 %
NACL 1%
MPS .05%
Perfume. 2%
Colour
Water to 100

RedPill

Member

August 7, 2019 at 2:36 pm

@Gunther Can we determine LABSA quality with its colour? I have seen Light transparent yellowish to Dark chocolate coloured LABSA.
Can we neutralize LABSA with Pottasium Hydroxide? (KOH) Is there any difference using than Sodium Hydroxide?
I have encountered seperation when adding TKPP with neutralized LABSA. Do you have any knowledge about this issue?

Gunther

Member

August 7, 2019 at 7:00 pm

Aziz said:

@Gunther

LABSA 8%
NaOH To pH 8.5
EDTA .2%
Na citrate .5%
SLES 4%
SLS 1%
TSP 1%
CDEA 3%
CAPB ( 30%) 4.5 %
NACL 1%
MPS .05%
Perfume. 2%
Colour
Water to 100

Add more SLES, but get rid of SLS
You can also add more LABSA with NaOH as required.
Some Ethoxylated alcohol helps with foam too.

Get rid of TSP as phosphates cause eutrophication of rivers and lakes and don’t add anything that LABSA or SLES doesn’t.

Did you cloud test this formulation?
“Cold weather Cloud Testing” can be as simple as putting the formulation in the fridge (without freezing) and see if it clouds on lower temps.
Lots and lots of beginner LABSA formulations cloud at low temps.

Get rid of salt and Na-citrate as they just rise cloud points.

RedPill said:

@Gunther Can we determine LABSA quality with its colour? I have seen Light transparent yellowish to Dark chocolate coloured LABSA.
Can we neutralize LABSA with Pottasium Hydroxide? (KOH) Is there any difference using than Sodium Hydroxide?
I have encountered seperation when adding TKPP with neutralized LABSA. Do you have any knowledge about this issue?

All 95%+ LABSAs I have seen are dark brown.
If it’s yellow then it’s either preneutralized, or diluted.

You can use KOH as it’s supposed to help rise cloud point temps.

I don’t like phosphates.
They cause eutrophication of lakes and rivers and don’t add anything useful to the formula that greener ingredients like LABSA, SLES or ethoxylated alcohols don’t.

Aziz

Member

August 8, 2019 at 1:53 am

Gunther said:

Aziz said:

@Gunther

LABSA 8%
NaOH To pH 8.5
EDTA .2%
Na citrate .5%
SLES 4%
SLS 1%
TSP 1%
CDEA 3%
CAPB ( 30%) 4.5 %
NACL 1%
MPS .05%
Perfume. 2%
Colour
Water to 100

Add more SLES, but get rid of SLS
You can also add more LABSA with NaOH as required.
Some Ethoxylated alcohol helps with foam too.

Get rid of TSP as phosphates cause eutrophication of rivers and lakes and don’t add anything that LABSA or SLES doesn’t.

Did you cloud test this formulation?
“Cold weather Cloud Testing” can be as simple as putting the formulation in the fridge (without freezing) and see if it clouds on lower temps.
Lots and lots of beginner LABSA formulations cloud at low temps.

Get rid of salt and Na-citrate as they just rise cloud points.

RedPill said:

@Gunther Can we determine LABSA quality with its colour? I have seen Light transparent yellowish to Dark chocolate coloured LABSA.
Can we neutralize LABSA with Pottasium Hydroxide? (KOH) Is there any difference using than Sodium Hydroxide?
I have encountered seperation when adding TKPP with neutralized LABSA. Do you have any knowledge about this issue?

All 95%+ LABSAs I have seen are dark brown.
If it’s yellow then it’s either preneutralized, or diluted.

You can use KOH as it’s supposed to help rise cloud point temps.

I don’t like phosphates.
They cause eutrophication of lakes and rivers and don’t add anything useful to the formula that greener ingredients like LABSA, SLES or ethoxylated alcohols don’t.

Yes I did the cloud test , without TSP and citrate it is stable at 4°C . And if Gsalt (Na₂SO₄ ) is used , cloud point increases .
I already deduct TSP and citrate . I added SLS for foaming . Then I tried with 1% AOS to achieve foam . It slightly increses foam .

I have two quality of LABSA , one is blackish and doesn’t give a clear and consistent dish wash and it was lower priced . A reddish one is fine , no issue with consistency , but I couldn’t achieve optimum foaming performance. My LABSA (96%) is not preneutralized , I neutraled it with NaOH . I know amine oxides are good for foaming but it is not available .
Oh another issue is some of the batches changing colour over time .

Gunther

Member

August 8, 2019 at 5:23 pm

@Aziz may I ask what’s the intended application?

If it’s for manual dishwashing
then a shampoo-like formula will work fine with much less irritation and cloudiness problems than LABSA.
SLES as the main surfactant, followed by a smaller amount of SLS (or neutralized LABSA), CAPB and even CDEA.

If it’s for liquid laundry or institutional dishwashing
Then LABSA 10-12%, SLES 4-8% and a small amount of CAPB (but not salt) will work fine.

Try to get the Certificate of Analysis from the suppliers to check their purities and concentration.
LABSA batches shouldn’t change color, and all those I’ve seen are dark brown, albeit with slighltly different hues.

Gunther

Member

August 9, 2019 at 6:38 pm

Maybe it is low quality LABSA is ladden with free sulfuric acid:

Linear alkyl benzene sulphonate obtained by sulphonation of LAB with sulphur trioxide gas contains minimum free sulphuric acid and is preferred to LABS obtained from oleum sulphonation that has a higher proportion of free sulphuric acid. Free sulphuric acid present precipitates as sodium sulphate increasing the inorganic content of the product and thereby reducing the

cloud point of the final product.
http://sitaramdixit.synthasite.com/resources/Laundry%20detergents%20-%20Moving%20from%20solid%20to%20liquid.pdf

Aziz

Member

August 10, 2019 at 12:08 am

Gunther said:

@Aziz may I ask what’s the intended application?

If it’s for manual dishwashing
then a shampoo-like formula will work fine with much less irritation and cloudiness problems than LABSA.
SLES as the main surfactant, followed by a smaller amount of SLS (or neutralized LABSA), CAPB and even CDEA.

If it’s for liquid laundry or institutional dishwashing
Then LABSA 10-12%, SLES 4-8% and a small amount of CAPB (but not salt) will work fine.

Try to get the Certificate of Analysis from the suppliers to check their purities and concentration.
LABSA batches shouldn’t change color, and all those I’ve seen are dark brown, albeit with slighltly different hues.

@Gunther It is for kitchen dish washing . Customers want ‘ Fairy ‘ like performance from it . Main purpose is to remove oil , fat , carbohydrates and dirt from dishes , plates etc. Now I am facing foaming performance .