DE1767808A1 - Process for making soap - Google Patents

Description

MY CHARACTERS;

UNILBVEH ff.V.
Museum Park 1, Rotterdam / Holland

Process for making soap.

Priority; British patent application Ho. 28 652/67 v. June 21, 1967

The invention relates to a method for producing Eife a ^UE, a ^UE UNAE particular Eife with improved color and improved Geruoh,

It is known that certain colored compounds which are present in minä erwertig en Letten or fatty acids are not removed by the usual treatment of old activated adsorbents. The characteristic öeruoh unparfitaierter ^ö ei * fe is dwaii treatment there d'setts or fettsäur · with an "activated adsorbent also difficult to remove. Ton the various possibilities of removing these colored and odorous compounds, which are not sufficiently sufficient

D (UTtCHt IANK A · ,, HARSUM Μ / Μ «« ΡΟ «Τ · ΟΗΒβΚ> HAMMUK · HTMSO TBUBPONIMOHB AMMAOHUNVBN BIOORPBN MCHRimiOHB * MBMTATIMUNM

109844/1347, I.

BATH ORIGINAL

Wise absorbed, some consideration seems to have been given to chemical reduction, however Nonselective reducing treatments, for example hydrogenation in the presence of a nickel catalyst, do not provide a useful solution because this has not yet been granted any great practical success Removal of color and odor results in an undesirable increase in the melting point of the fat deposits. Furthermore are special pressure vessels necessary to carry out the hydrogenation

Certain reducing agents, such as alkali metal borohydrides, decompose known, at higher temperatures in aqueous ¹¹ solution, in which the rate of decomposition increases with increasing temperature and with increasing alkalinity of the solution · decreases contrast, it was surprisingly found that low concentrations τοη alkali borohydride quickly the coloring and the odor a viscous medium such as melted soap can reduce

Accordingly, the invention provides a method of making a soap, which is the treatment of a soap-based system in any manufacturing stage with one JLLkaliborhydrid at a pH τοη Includes at least 9.5.

The color of the soap obtained by this process is usually measured on a 5 »84 g / 100 cm ⁵ aqueous solution of the soap (^ roeken base) with the aid of a Lovibond tintometer using a

109844/1 347

Lovibond measured 15.3 cm cell. The acceptable color depends on the intended use of the soap produced « The color is determined in Lovibond red and Lovibond yellow units. These units are combined to one value, which in the description is called soap color and using the formula

Soap color = 10 χ (yellow number) + 3Ox (red number) is obtained.

As used herein, the term "soap base" refers to the material obtained by saponifying a suitable base of fat and alkali. The expression "fat" can refer to animal sebum, a vegetable oil such as palm oil, palm kernel oil or coconut oil, a fish oil or to the fatty acids obtained from such substances by a conventional cleavage process. Mixtures of these fats can also be used in the process of the invention. A common mixture consists for example of IaIg and up to 20 wt. $ Of an oil such as coconut oil · These fats are referred to as "fat approach" · When the rich approach is inferior, it should be with a bleaching earth or any other adsorbent bleaching agent (in hereinafter referred to as a standard bleaching treatment) be pretreated before saponification «so that the bo removable paint cannot consume borohydride · The color of a bleached inferior sebum can range from 4.0 yellow, 0.8 red to 15.0 yellow, 2.5 red ( measured in a 0.635 * I «ovibondBelle) fluctuate

Synthetic acidic acid. which e.g. by oxidation obtained from paraffinic hydrocarbons,

ORIGINAL INSPECTED

can also be used alone or in a mixture with a fat in the process according to the invention.

A soap mixture from a bleached toilet soap tallow or the soap obtained from it can also be used the method according to the invention are treated, in particular when it is desired to obtain a product substantially free of odorous compounds.

The term "alkali" used in the following is intended to refer to lithium, potassium or sodium. Of the Alkali borohydrides are the easiest of the sodium derivatives commercially available · The alkali borohydride can either be in solid form in the process according to the invention or as an aqueous solution or as a mixture with soap. It can also be in situ from others Borohydrides are formed · Preferably it is added as a solution in aqueous alkali, being a suitable alkali is sodium hydroxide or potassium hydroxide.

^M in situ formation of an alkali borohydride is understood to mean the addition of a borohydride salt other than an alkali salt to a soap-containing system. As a result of the large excess of alkali metal ions which are present in such a system, the borohydride salt is converted into the alkali borohydride The alkali borohydride is expediently added either at the end of the saponification or after the completion of the saponification, since at this point in time the pH of the system does not fluctuate as much as at the beginning of the saponification.

109844/1347

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If the boron hydride is added during the saponification stage ; the system should continue to boil for about another 50 minutes to complete Ensure dispersion of the borohydride and strongest reduction in the color and odor of the soap base. The total elimination of color and odor depends on the effective distribution of the borohydride in the System and the amount used.

Color and odor removal can also be done after completion Saponification can take place while the soap is still liquid enough to allow sufficient mixing with the borohydride and so long as the pH of the soap does not drop below about 9.5, a preferred range of pH is between 9.5-14.0.

The alkali borohydride is preferably used immediately after washed the soap resulting from the saponification process was added to the soap or just prior to drying. But it is also possible to use the borohydride Add soap immediately after drying or in the piling stage (with simultaneous addition of pigment).

The temperature of the soap system must be controlled and there must be sufficient alkali in this system so that there is enough time for the borohydride to be fully dispersed and for the reduction to occur before its decomposition. 100 ⁰ O is added, the pH should preferably be 1.0-14 »0. In continuous or semi-continuous processes, in which a more effective ^

"*" 109844/1347 copy

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If constant mixing is used, the pH control need not be quite as strict.

The improvement of the color and smell of ^ö Eife applied amount of alkali metal borohydride, preferably lies within the range 0.005 to 0.30 wt $ 6 of the total fatty acid content of the soap used.. A particularly preferred amount of borohydride for treating a soap obtained from standard bleached sebum for toilet soaps is within the range of 0.02-0.10% by weight of the fat base. The addition of borohydride to more than 0.30% by weight of the fat addition is naturally also effective but uneconomical.

Borohydrides decompose in an aqueous medium with the formation of borate ion and hydrogen. Adequate precautionary measures should therefore with regard to the risk of fire associated with the development of hydrogen and the associated problem of foam formation. The foam formation can be regulated by

a) Gradual addition of the borohydride to the soap-containing one System in a vessel with sufficient volume to allow any expansion of the soap-containing system enable, or

b) adding the borohydride to the soap immediately before pumping the soap into a dryer, and keeping the soap in that dryer under pressure until it is on another treatment apparatus (e.g. a vacuum chamber or a cooling drum) is sprayed, or

c) adding the borohydride to the Seif · when it leaves the scrubber and Entgaeen duroh spraying the treated ^ö Eife in the Absetzbehftlter.

1098U / iUf

BATH ORIGINAL

1767908

The borate ion is easily removable from the treated soap by washing with water, even though its presence is no adverse effect on the ^above Eife or other material (such as a perfume) exerts, which is to be to the ^UE Eife in a later stage of its manufacture added. A further advantageous feature of the process of the invention lies in the Umetand that it can be applied easily mm in a normal soap making procedures. Fireproofing the ^above eifenherStellungsmaschinerie, in view of the possible ffefahren which is smaller with the development of hydrogen amounts are connected, may be necessary.

The amount of adsorbent used in the standard bleaching treatment an inferior fat base is preferably about 6 öew.ji of the fat base. Fuller's earth is a preferred bleaching agent, but other adsorbent earths or lead carbon can also be used.

Color and odor of the treated ^b Eife depends on the amount and type of adsorbing bleaching agent which is optionally used in the pretreatment of the fat layer, the amount of used alkali metal borohydride, the time and temperature of treatment with the borohydride, the pH of the soap-containing Miechung during the borohydride treatment and the effective mixing of the soap-containing system

Another advantageous effect, which is obtained when the borohydride is added during the saponification stage, is that the glycerine base liquor produced is almost as bright as a vase.
1098U / 1347

8AD ORIGINAL

The invention will be further explained with reference to the examples. example 1

Bin inferior tallow was mixed with four different percentages (of 1-6 Gew.96) Pullererde for 5 minutes at 105-11O ⁰ C and additional 5 minutes at 110-115 ⁰ C treated "After filtering off from the Pullererde were obtained from the tallows Each of the four bleaching trials was divided into three aliquots in beakers, each aliquot containing 20 parts by weight of bleached sebum. After melting these sebum samples on a boiling water bath, 10 parts by volume of a 30 g / 100 cn aqueous sodium hydroxide solution were added to the first sample of each bleaching experiment, these mixtures were kept on a boiling water bath and stirred until complete saponification. 9 parts by volume of 30 g / 100

cm sodium hydroxide solution was added to the remaining added two samples from each bleaching experiment. These mixtures were then saponified in the same way

40 minutes after adding the sodium hydroxide solution 1 part by volume of 30 g / 10 og cm of aqueous sodium hydroxide solution containing 0.01 part by weight of sodium borohydride was added to the second sample each with stirring Added bleached sebum to be saponified · By volume of 30 g / 100 car of aqueous sodium hydroxide solution, which contained 0.02 parts by weight of sodium borohydride, was in added in the same way to the third sample of each of the bleached tallow to be saponified

109844/1347 originally inspected

After one hour, 10 parts by volume of water to leather were added to the 12 saponified samples and the resulting mixtures were homogenized by rapid stirring. The homogenized mixtures were then transferred to a large beaker ·, 290 parts by volume of distilled water added to each and the soap by heating to about 75 ⁰ C dissolved the color of each of the obtained solutions was determined by soap Lovibondkolorimetrie in a 13.3 cm cell "The results obtained follow in the! table

$> Fuller's earth

f> sodium
bor hydrated 0 0.05 0.1 0 O, 05 0 , 0 0.05 2 0 O, 05 0 ,1 Lovibond yellow 29 27 15th 7, 4 6 , 3 4th ,8th 3.2 0 > Q 1, 5 1 , 5 Lovibond red 1.0 1.0 0.8 1, 5 1 , 0 0 0.6 , 6 O, 3 0 , 2

Example 2

A fat batch of 92.5 Gew _e # sebum, which had been bleached by treatment with 6 Gewe # adsorbent soil and had a Lovibond Yellow Number of 11.7 and a Lovibond Red Number of 1.4 in a 5.1 cm cell, and from 7.5 wt% _e coconut oil, ° C was saponified in a conventional soap boiler · si the soap produced was separated from the substrate solution and washed in a conventional washing vessel with a 1 g / 100 cm sodium hydroxide containing liquor at 95th When the washed soap came out of the washing vessel, it was treated with an amount of aqueous 5.0 g / 100 cm sodium hydroxide solution containing 10% by weight of sodium borohydride

109844/1347

ORIGINAL INSPECTED

I / 67808

sufficient to 0.1% sodium borohydride, based on the The weight of the originally "" saponified fat deposit should be provided. The borohydride-treated soap was then allowed to settle, neutralized and heated and dried according to standard technology The soap color of a soap treated in this way was 37% the soap color of a soap, obtained from the same fat mixture, which was not treated with borohydride, 60 was.

In a further experiment, the soap was washed with a lye which contained 2 g / 100 cm of sodium hydroxide. The soap color of untreated soap was 54 · The color of the soap, which was treated with 0.1 · $> sodium borohydride was 43 ·

When borohydride was applied, hydrogen evolution inflated the 20 tons of soap made in each of the above experiments to a volume that would otherwise have been occupied by 35 tons of soap. Example 3

A fat batch of 92.5% by weight of tallow which had been bleached by treatment with 6% by weight of absorbent soil and had a Lovibond Yellow Index of 6.0 and a Lovibond Red Index of 0.9, as measured in a 5.1 cm cell, and from 7.5 wt.% Coconut oil was at 95 ° C in a conventional Soap kettle saponified. The soap prepared in this way was separated from the lower liquor and then with a Washed lye, which contained 1 g / 100 carbons of sodium hydroxide. Aqueous 5 g / 100 cnr sodium hydroxide solution,

109844/1347

ORIGINAL INSPECTED

Chilling 10 wt. sodium borohydride (in an amount sufficient to provide 0.02 wt. The soap color of the soap treated in this way was 26 = (1.4 ^δ ? 1Ϊ4 red). The soap color of the remaining soap, which had not been treated with sodium borohydride, was 39 = (2.1 yellow +0.6 red)
Example 4

A 1.9 ton soap batch was made by saponifying one Fat base composed of 85% by weight of tallow and 15% by weight of coconut oil · The lower lye was separated from this soap mixture and the soap was washed with a lye which contained 1 g / .tQQ cnr sodium hydroxide, allowed to settle and sent through heat exchangers before drying, forming and extrusion Sodium borohydride was in a cold aqueous 4 g /

■ χ
100 car sodium hydroxide solution with a sufficient

Amount dissolved to provide 15 g / 100 cm ³ solution. A sufficient amount of this solution was applied to provide an amount of borohydride equal to 0.1 wt% of the fat base. This solution was injected into the soap line immediately before the pump feeding the heat exchanger for 30 minutes "- samples of the treated soap were taken after drying, piling and extrusion and checked for free alkalinity and soap color.

1098U / 1347

ORDINAL JNSPECTED

checks.
template

- 12 -

Free alkalinity color% Na ₂ O yellow

none 2.0 0.01 2.4

Red

0.5 0.5

(untreated)

0.04 0.01 0.04 0.03

1.4 1.3 1.5 1.6

0.3 0.2 0.3 0.3

(treated)

no

2.0

0.4 (untreated)

The annoying foaming was to a large extent overcome by this method « Example 5

A 113 kg fat base made from 80% by weight of bleached material toilet soap tallow and 20 Gewo # standard bleached products Coconut oil was rerseifto The soap obtained in this way was separated from the lower liquor, washed and allowed to settle · This soap had a free alkali retention τοη 0.01 ^ ·

Sin 18 kg sample of this soap was heated to 90 ⁰ C. 750 ml of a 10 percent strength by weight sodium borohydride solution in aqueous 5 g / 100 cmr sodium hydroxide solution were gradually added to the heated soap while stirring, which constituted an addition τοη 0.1? Ί sodium borohydride, based on the weight of the fat present in the soap. Another 420 ml aqueous 5 g / 100 car sodium hydride solution

, solution, reducing the amount of free alkali to 0.5 ^ weight / volume

1098U / 1 3 Λ 7

ORIGINAL JNSPECTED

was increased were added even to the soap-containing system, to the extent of foaming to verringern.Ein further 18 kg pattern of the borohydride was in the same manner _ith half the volume treated.

The treated soap was allowed to settle piliert and extruded and evaluated their color from a group of knowledgeable persons who were asked to smell the soaps with closed eyes to exclude so any influence of color differences, and to comment on ^what's Eife the has a stronger smell. Since the samples were not perfumed, the findings of the group of people were a direct measure of the strength of the unwanted basic odor. Each odor was scored +1 for the bars with the stronger odor, 0 for no difference and -1 for those having the weaker odor. The scores from each person for each soap were added to give a total score for any soap to get there. Ert a low ^w shows little cause odor and a high ^w ert of strong base odor.

The test samples also contained pieces of soap, which were irrelevant for the invention, and the The results of this soap bar were disregarded. The odor values for each individual row were therefore not around zero as the middle, how let it in a full Muatervergleioheanalyse should have gttan

109844/1347

Addition of borohydride. Odor value

- (control) +13.2

0.05 * -12.7

0.1% -39.8 standard error ± ¹⁵ » ⁷

The difference in the double standard error is characteristic of a 5% probability · Example 6

Another 18 kg pattern of soap, prepared in Example 5, was heated to 9O ⁰ C, "880 ml of a 10 weight percent Kaliumborhydridlösung in aqueous 5 g / 100« m sodium hydroxide solution was gradually added to the soap with stirring to an addition of 0 08% by weight of potassium borohydride, based on the weight of the fat deposit, made up an additional 320 ml of aqueous 5 g / 100 cm ^ sodium hydroxide solution, which increased the amount of free alkali to 0.5 g / 100 cm ⁵ , was added to the soap added to reduce foaming. This experiment was repeated with three further 18 kg samples of the soap prepared in Example 5, with the modification that the amount of potassium borohydride solution added was reduced. The amounts of potassium borohydride used in each pail were 0.02%, 0.04% and 0 , 06% of the weight of the fat depositThe odor value of each sample was tested as follows:

109844/1347 originally inspected

A group of 10 people were asked to smell samples of the after the procedure For example, compare treated soaps with a sample of untreated soap and compare each sample according to the degree achieved in their opinion Classify deterioration. The following table shows the number of people who were able to

to correctly indicate the correct position of each pattern.

• borohydride No of the right position 0 10 0.02 7th 0.04 8th 0.06 7th 0.08 8th

109844/1347

Claims (1)

-16- 1/67808 Claims 1, Veranrei: for making soap, thereby geke υ η draws that the ^ maturity or a üeifenansc.tz in any stage of production dor ⁰ CiTe uit an alkali borohydride at a pH of ininaei: at least 9.5 treated \ virdo 2 c PROCEDURE ": NaCN claim 1, characterized ge e ic η η - η c ζ calibration ΐ that the ^ Eife eiitz from Einein Pettan- whose Hauptbe £ ta2idteil sebum is produced ir ν α". 3 «Method according to claim 2, characterized in that g e k e η η draws that the fat deposit is pretreated with an adsorbing bleaching agent, 4o procedure according to claim 2 or 3, thereby marked that the ^ maturity with the Ali: aliborh "drid after the saponification of the fat deposits treated v.'ird. ^ - · Method according to the preceding claims, thereby marked that s the Soap miö dee Alkalibornydric. immediately after her Washing is treated. 6 ο method according to the preceding claims, thereby marked that the ° eife or the soap preparation with a certain amount of alkali borohydride equal to 0.01-0.30 wt.% of the fat deposit treated v: irä. 1098AA / 1347
BATH 7 ο Veri "£: .o.iren nacxi the preceding * -nsgv'J.ciion, characterized in that üie soap or the ^D eifenansatz is traded with the alkali metal borohydride as a solution in aqueous alkali. 8. Method according to the preceding Ans ρ-.ilen eh, characterized in that the bang with eggs alkali borohydride unxSÄxMsx ^ SK Ha the passage in a dryer is treated. 1098A4 / 13A7 BATH ORIGINAL