EP4698620A1

EP4698620A1 - Biosurfactant composition and method of preparation thereof

Info

Publication number: EP4698620A1
Application number: EP24792289.1A
Authority: EP
Inventors: Vardharaj Petkar MANISH; Karthickeyan A; Pillai S. SIVARAMAKRISHNA
Original assignee: Proklean Technologies Pvt Ltd
Current assignee: Proklean Technologies Pvt Ltd
Priority date: 2023-04-20
Filing date: 2024-04-17
Publication date: 2026-02-25
Also published as: WO2024218791A1; KR20260007194A

Abstract

Disclosed is a biosurfactant composition includes guerbet alcohol salts ranging from 10- 20 % (wt/wt) of the biosurfactant composition, lauryl alcohol salts ranging from 15 to 25 % (wt/wt) of the biosurfactant composition, protein hydrolysate ranging from 1 to 5 % (wt/wt) of the biosurfactant composition; glycerine ranging from 1 to 5 % (wt/wt) of the biosurfactant composition; extracts of soap nut (Sapindus mukorossi) ranging from 1 to 5 % (wt/wt) of the biosurfactant composition; and wherein upon homogenization provides an emulsion index in the range of 60-70% The present disclosure further discloses a method of preparation of the biosurfactant composition.

Description

BIOSURFACTANT COMPOSITION AND METHOD OF PREPARATION THEREOF

TECHNICAL FIELD

The present disclosure relates to biosurfactants. More particularly, the present disclosure relates to a biosurfactant composition and method of preparation of the biosurfactant composition.

BACKGROUND

Surfactants are organic compounds consisting of at least two parts, one is the lyophobic part which is insoluble in a specific solvent and other is lyophilic part which is soluble. This dual character of surfactant makes it amphipathic in nature. There are different kinds of surfactants, but mostly cationic, anionic and non-ionic are predominantly used in the various industrial applications.

Surfactants constitute one of the important parts of several products like personal care products, detergents etc. Detergents serve as an efficient cleaning product because it is made up of one or more surfactants along with other chemicals. Apart from the being used in personal care and detergent formulations, surfactants have their applications in various other fields like oil recovery processes, in production of food items where the surfactants are used in solubilization of oil, liquor emulsification, extraction of cholesterol. Its applications are vast, including in the field of agriculture where surfactants are used to decrease the surface tension of the spray solutions of herbicides, pesticides etc.

Surfactants are the inherent part of the consumer formulations. The present market for consumer range of products is mainly produced from category of surfactants including sodium lauryl sulphate (SLS), sodium lauroyl sarcosinate (SLS), sodium dodecyl sulphate (SDS), and cocomidopropyl betain. One of the key concerns of all these surfactants is lack of skin friendliness which is an important requirement of all the consumer products. Lesser the skin friendliness higher is the skin damage on a longer use of these products. Most of the consumer formulations available in the market are chemical based surfactants which are used in the concentration range of 10-25 % in formulations. The higher concentrations of above 20% surfactant are proven to have low skin friendliness. Moreover, some chemical surfactants have strong cleansing effect where it results in removal of natural oils from the skin and cause dryness, discomfort, and allergic reactions to the skin. Apart from the disadvantages mentioned above, other important environmental concerns with respect to chemical surfactants are its poor biodegradability and low renewable carbon content. Though, chemicalbased surfactants might provide consistent and stable emulsification performance due to their amphiphilic nature (having both hydrophobic and hydrophilic components), but they have a higher environmental impact due to the production of petrochemicals, also making it non-appealing ingredient for skin and personal care products. Moreover, the surfactants available in the current state of art with increased viscosity experience disadvantages such as operational difficulties during manufacturing of raw materials, altered deliverables of the final product (personal care or home care products) and stability issues of the developed end product formulation.

Over the past two decades, new surfactant molecules have been appearing at a relatively rapid pace. Scientific curiosity has also driven surfactant science research to focus on surfactant molecules having interesting, fabricated shapes, structures, properties and uses.

Several prior arts discuss surfactant compositions like the patent application US20100009892A1 titled as “multi-function surfactant composition” discusses a surfactant concentrate which is an admixture of a phosphonated amphoteric surfactant and a fluor surfactant. The phosphonated surfactant may be used alone or in admixture with a second phosphonated surfactant, an additional amphoteric surfactant or a Zwitterionic surfactant. The discussed multi-functional surfactant concentrate comprises a phosphated amphoteric surfactant, a fluorinated surfactant and water.The said surfactant composition may be used to formulate either a highly caustic detergent concentrate or an acid cleaner, which can have a greater cleaning effect, but low skin friendliness. Another patent application US20200060951A1 titled as “High- Concentrate Flowable Liquid Anionic Surfactant Composition” discusses a high- concentrate flowable liquid anionic surfactant composition which remains flowable when diluted with an aqueous solvent; and a method of reducing the viscosity increase of a high-concentrate liquid anionic surfactant composition when diluted with an aqueous solvent. Yet another application US4256605A titled as “Surfactant composition and concentrate and emulsion including same” discusses novel compositions which are useful as surfactants for the emulsification of oils in aqueous media. It also relates to oil-in-water type emulsions which incorporate the novel compositions. The invention primarily discusses compositions useful as surfactants in the emulsification of oils in aqueous media are obtained by blending two types of polyesters.

The prior arts mentioned in the state of art are chemical based and none of them discuss a biodegradable formulation. Though several prior arts discuss the surfactant concentrate compositions, none of the prior art discusses a unique skin friendly biobased composition (skin solubilization of surfactant is not more than 5%).

Accordingly, there exists a need for a bio-based surfactant composition which is biodegradable, skin friendly, antimicrobial and eco-friendly that also exhibit better results in terms of emulsification ability.

SUMMARY OF INVENTION

In one aspect of the present disclosure, a biosurfactant composition is provided.

The biosurfactant composition includes guerbet alcohol salts ranging from 10- 20 % (wt/wt) of the biosurfactant composition. The biosurfactant composition further includes lauryl alcohol salts ranging from 15 to 25 % (wt/wt). The biosurfactant composition further includes protein hydrolysate ranging from 1 to 5 % (wt/wt). The biosurfactant composition further includes glycerine ranging from 1 to 5 % (wt/wt). The biosurfactant composition further includes extracts of soap nut ranging from 1 to 5 % (wt/wt).

In some aspects of the present disclosure, the biosurfactant composition further includes water ranging from 50-70% (vol/vol) of the biosurfactant composition.

In some aspects of the present disclosure, the guerbet alcohol salts are selected from a group which includes guerbet alcohol ethoxylates or derivatives thereof.

In some aspects of the present disclosure, the lauryl alcohol salts are selected from a group comprising alcohol ethoxylates or derivatives thereof.

In some aspects of the present disclosure, the soap nut extract used is Sapindus mukorossi.

In some aspects of the present disclosure, the said biosurfactant composition upon homogenization provides an emulsion index in the range of 60-70%.

In the second aspect of the present disclosure, a method of preparation of biosurfactant composition is provided.

The method includes mixing protein hydrolysate with water in a beaker to obtain an aqueous solution of protein hydrolysate. The method further includes stirring the aqueous solution. The method further includes adding glycerol to the aqueous solution followed by agitation to obtain the first mixture. The method further includes adding aqueous solution of soap nut extract to the mixture to obtain the second mixture. The method further includes adding guerbet alcohol salts and lauryl alcohol salts to the mixture to obtain the biosurfactant composition mixture.

In some aspects of the present disclosure, the biosurfactant composition is further made up to a desired volume and concentration by adding water. In some aspects of the present disclosure, the method is performed in a stirring condition to obtain homogeneity.

BRIEF DESCRIPTION OF THE ACCOMPANYING GRAPHS:

The accompanying drawings, which are incorporated in and constitute a part of this specification, show certain aspects of the subject matter disclosed herein and, together with the description, help explain some of the principles associated with the disclosed implementations. In the drawings-

Figure 1 illustrates a flowchart that depicts a method of preparation of the biosurfactant, in accordance with an aspect of the present disclosure; and

Figure 2 illustrates an image representing resultant emulsion layer and biosurfactant, in accordance with an aspect of the present disclosure.

DETAILED DESCRIPTION:

Various embodiments of the disclosure are discussed in detail below. While specific implementations are discussed, it should be understood that this is done for illustration purposes only. A person skilled in the relevant art will recognize that other components and configurations may be used without parting from the spirit and scope of the disclosure. Thus, the following description and drawings are illustrative and are not to be construed as limiting. Numerous specific details are described to provide a thorough understanding of the disclosure. However, in certain instances, known details are not described in order to avoid obscuring the description.

References to one or an embodiment in the present disclosure can be references to the same embodiment or any embodiment; and such references mean at least one of the embodiments.

Reference to "one embodiment", "an embodiment", “one aspect”, “some aspects”, “an aspect” means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment of the disclosure. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments. Moreover, various features are described which may be exhibited by some embodiments and not by others.

A recital of one or more synonyms does not exclude the use of other synonyms. The use of examples anywhere in this specification including examples of any terms discussed herein is illustrative only and is not intended to further limit the scope and meaning of the disclosure or of any example term. Likewise, the disclosure is not limited to various embodiments given in this specification. Without intent to limit the scope of the disclosure, examples of instruments, apparatus, methods and their related results according to the embodiments of the present disclosure are given below. Note that titles or subtitles may be used in the examples for convenience of a reader, which in no way should limit the scope of the disclosure. Unless otherwise defined, technical and scientific terms used herein have the meaning as commonly understood by one of ordinary skill in the art to which this disclosure pertains. In the case of conflict, the present document, including definitions will control.

Additional features and advantages of the disclosure will be set forth in the description which follows, and in part will be obvious from the description, or can be learned by practice of the herein disclosed principles. The features and advantages of the disclosure can be realized and obtained by means of the instruments and combinations particularly pointed out in the appended claims. These and other features of the disclosure will become more fully apparent from the following description and appended claims or can be learned by the practice of the principles set forth herein. As discussed before, there exists a need for a bio-based surfactant composition which is biodegradable, skin friendly and eco-friendly that also exhibit better results in terms of emulsification ability. Therefore, the present disclosure provides: a biosurfactant composition with reduced surface tension that provide a skin friendly surfactant able to penetrate the skin more readily, facilitating the absorption of active ingredients, thereby providng improved cleansing suitable for delicate skin types.

The present disclosure provides a biosurfactant composition with better emulsification ability, where the formulation’s ingredient selection and concentration is optimized which is substantial to achieve the stable emulsification index value.

The present disclosure provides a biosurfactant composition, that identifies the raw materials and the concentration effects that contribute for a higher deviation in the overall viscosity, foaming property of the end formulation and evaluation of their performance parameters.

The biosurfactant composition includes guerbet alcohol salts, lauryl alcohol salts, protein hydrolysate, glycerin, soap nut extract.

In some aspects of the present disclosure, the guerbet alcohol salts ranges from 10 to 15 % (wt/wt) of the biosurfactant composition.

In some aspects of the present disclosure, the lauryl alcohol salts ranges from 15 to 20 % (wt/wt) of the biosurfactant composition.

In some aspects of the present disclosure, the protein hydrolysate ranges from 1 to 5 % (wt/wt) of the biosurfactant composition.

In some aspects of the present disclosure, the glycerin ranges from 1 to 5 % (wt/wt) of the biosurfactant composition. In some aspects of the present disclosure, the soap nut extract ranges from 1 to 5 % (wt/wt) of the biosurfactant composition.

In some aspects of the present disclosure, the biosurfactant composition further includes water that ranges from 50-70% (vol/vol) of the biosurfactant composition.

In some aspects of the present disclosure, the guerbet alcohol salts are one of, but are not limited to, guerbet alcohol ethoxylates or derivatives thereof and the like. Aspects of the disclosure are intended to include known and later developed guerbet alcohol salts.

In some aspects of the present disclosure, the lauryl alcohol salts are one of, but are not limited to, lauryl alcohol ethoxylates or derivatives thereof and the like. Aspects of the disclosure are intended to include known and later developed lauryl alcohol salts.

In another aspect of the invention, upon homogenization said biosurfactant composition, provides an emulsion index in the range of 60-70%.

Figure 1 illustrates a flowchart that depicts a method (100) of preparation of the biosurfactant composition, in accordance with an aspect of the present disclosure. The method (100) includes the following steps:

At step (102), the method (100) includes mixing protein hydrolysate with water in a beaker to obtain an aqueous solution of protein hydrolysate.

At step (104), the method (100) includes stirring (104) the aqueous solution obtained at step (102).

At step (106), the method (100) includes adding (106) glycerol to the aqueous solution obtained at step (104) followed by agitation to obtain a first mixture.

At step (108), the method (100) includes adding (108) aqueous solution of soap nut extract to the mixture obtained at step (106) to obtain a second mixture. At step (110), the method (100) includes adding guerbet alcohol salts and lauryl alcohol salts to the mixture obtained at step (108) to obtain the biosurfactant composition mixture.

In some aspects of the invention, the method (100) is performed in a stirring condition to obtain homogeneity.

In some aspects of the present disclosure, the biosurfactant composition obtained at step (110) is further made up to a desired volume and concentration by adding water.

In some aspects of the present disclosure optimized concentration provides higher surface tension reduction.

EXAMPLES:

Preparation of biosurfactant composition

0-5%(w/w) of protein hydrolysate was added in a beaker having water followed by stirring and an aqueous solution of protein hydrolysate was obtained. 0-1.5% (w/w) of glycerine was added to the obtained aqueous solution of protein hydrolysate followed by agitation and a first mixture was obtained. 0-5% of soap nut extract was added to the first mixture and the second mixture was obtained. 0-15% (w/w) of guerbet alcohol salts and 0-20%(w/w) of lauryl alcohol salts were added to the second mixture and the biosurfactant composition was obtained.

Example 1: Studies on impact on surface tension

The ability of the products of the biosurfactant composition to reduce the surface tension of water were analyzed in the given study.

Example 1.1 Procedure for finding the surface tension of the sample biosurfactant.

25 ml of sample was taken in a clean and dry measuring beaker. Further, select the appropriate spindle from the viscometer accessories. Attach the spindle in the viscometer and run the spindle as per the method prescribed for the spindle size. Further, note down the surface tension reading and repeat the process with water to calculate the reduction in surface tension.

The initial surface tension of water was measured as 72 mN/m. The individual ingredients were tested to assess the surface tension, as well as the surface tension of biosurfactant composition was measured.

Table 1 provides the details on the observed values regarding the surface tension with the ingredients and biosurfactant composition.

Generally, an ideal surfactant exhibits low surface tension values. The individual surface tension values observed range from 0-46mNm. From the given table the average calculated value of the surface tension of these components is observed as 44.2mNm. The optimized biosurfactant composition exhibits synergistic results, where the surface tension value is reduced to 31mNm.

Thus, it was inferred that the individual RM surface tension reduction is random and low in the case of all the RMs. Further, the formulation ingredient selection and concentration is optimized to get the final reduction with higher surface tension reduction than individual RMs. The higher surface tension reduction implicates the effectiveness of the formulation.

Example 2: Estimation of emulsification index value (E24)

Example 2.1: Preparation of control

0.5ml of Triton X-100 was added to tube containing 3.5ml of distilled water. 4ml of hydrophobic base was added to the test tubes (Note: The test tubes were agitated by way of vortex mixture for 2 minutes and left undisturbed for 24 hour). The emulsification index was calculated by calculating the heigh of emulsion layer with total height of the mixture.

Example 2.2 Procedure for finding the Emulsifying index of the sample biosurfactant

4ml of biosurfactant was added to the test tubes. 4ml of hydrophobic base was added to the test tubes. The test tubes were agitated by way of vortex mixture for 2 minutes and left undisturbed for 24 hours. An emulsion layer was obtained in each test tube (as shown in figure 2).

The emulsification index was calculated by calculating the height of emulsion layer with total height of the mixture. The obtained results were compared against a triton X-100 which is a control.

Example 2.3 Calculation of emulsification index

In the test tube containing biosurfactant, the total height was observed as 5.5 and the height of the emulsion layer was observed as 3.2. [as per the formula, Emulsification Index (El) % = (Height of the Emulsion Layer / Total height of the mixture) * 100].

Emulsification Index (E24) = (3.2/5.5) *100 = 58.18% In the test tube containing control (Triton X-100), the total height was observed as 5.3 and the height of the emulsion layer was observed as 3.6. Therefore, the emulsion index is calculated as (3.6/5.3) *100 = 67.92%

Therefore, on comparison to the standard, the emulsification ability of product is - (58.18/67.92)* 100= 85.65%

Table 2 provided below represents the values for Emulsion index values obtained for individual ingredients and the biosurfactant composition.

It was observed that the individual surfactants showed E24 % value but the natural plant-based ingredients have resulted in nil value. The biosurfactant composition which exhibited synergistic results with a higher emulsion index value of 55. Further, it is observed that the formulation ingredient addition sequence and concentration is optimized in a way to get the final formulation with stable E24 %. The higher E24 is required for the effective emulsion nature of the final formulation. The plant based RMs blending is essential as it makes the final formulation more skin friendly. The final biosurfactant composition has provided an emulsification ability whose E24(%) value is 55 which is double the value of the average individual components, confirming its efficiency.

Example 3: Experimental Studies on Viscosity

Experiments were conducted in varying concentrations of ingredients for the biosurfactant composition. More particularly, there were 2 sets of studies:

The first set of the study involved eliminating each raw material in separate variants of the original biosurfactant composition. Further, each variant was tested for the key performance parameters including viscosity and foam which are one of the key parameters for assessing the efficiency of any surfactant (Note: Viscosity and foam height are measured using standardized experiments viz standard viscometer

(A1S@5ORPM) and Ross miles test respectively)

The second set of studies involved evaluating the concentration effect of the key surfactants on the performance parameters.

The details of the experiments are as follows - Table 3 indicates first set of study for the effect of individual RM (raw materials/ components) in the formulation deliverable that discusses the formulations of El -E5 studied. were taken to prepare the biosurfactant composition, with at least one ingredient deficient in each of the formulations E1-E5.

Table 4 indicates the results in terms of viscosity and foam height. From Table 4, it is inferred that the presence of the ingredients Gubert alcohol Ethoxylate and Lauryl alcohol Ethoxylate has a significant impact on the formulation viscosity as observed with increased values in E-3 to E-5.

The second set of study is indicated in Table- 5, referring to impact of Gubert alcohol and Lauryl alcohol ethoxylate in the formulation. As provided in Table 5, for the second set of study varying concentrations of Gubert alcohol and Lauryl alcohol ethoxylate were used, and the concentration of the ingredients Saponin extracted from soap nut, Protein hydrolysate and Glycerin were unchanged for the formulations E6-E9.

Table 6 indicates the results in terms of viscosity and foam height in relation to formulation E6 TO E9

From results provided in Table 6 it is inferred that increasing or decreasing the concentration of Gubert alcohol ethoxylate and Lauryl alcohol ethoxylate, has a significant impact on the formulation viscosity. Further, with respect to Gubert alcohol ethoxylate, both increased and decreased concentrations have resulted in same increased viscosity. Further, with respect to Lauryl alcohol ethoxylate, increasing the concentration resulted in increased viscosity and reduced concentration has resulted in reduced viscosity.

Example 4: Impact analysis of the End Product Formulation:

In order to validate the impact of the above mentioned biosurfactant composition, a handwash prototype was formulated as an end product formulation with possible variants. The observations are as follows as provided in Table 7 and Table 8:

Example 4.1 Observations for Set I study:

Table 7 provides the impact of the end product formulation with reference to El to E5 in terms of hand feel, easy rinse and foam generation.

Note: More the “+ ” sign indicates better the performance

From Table 7, actual value of the biosurfactant composition exhibited an overall performance. Further, it is inferred that the formulation E2 and E4 exhibited a higher viscosity. In terms of the significant impact on hand feel, easy rinse and foam generation better performance was also exhibited by E-4 (concentration of the ingredients refer

Table 3) in comparison to other formulations. E-l to E-5 exhibited similarity in easiness to rinse.

Example 4.2. Observations for Set II study:

Table 8 provides the impact of the end product formulation with reference to E-6 to E- 9 in terms of hand feel, easy rinse and foam generation.

Note: More the “+ ” sign indicates better the performance The biosurfactant composition actual value in terms of viscosity was observed as 420, exhibited an overall higher performance in hand feel, easy rinse and foam generation. The formulations E-6 and E-7 exhibited an increased viscosity with reduced hand feel and easy rinse. E6 exhibited better foam generation alone whereas E-8 and E-9 exhibited phase separation.

The results indicate that the biosurfactant composition is unique in terms of its ingredient selection and concentration of the individual ingredient which results in an optimized formulation with desired deliverables. The alterations in the composition of the formulation will result in lesser stability, poor performance deliverables and complicated operational handling due to higher viscosity.

The implementation set forth in the foregoing description does not represent all implementations consistent with the subject matter described herein. Instead, they are merely some examples consistent with aspects related to the described subject matter. Although a few variations have been described in detail above, other modifications or additions are possible. Further features and/or variations can be provided in addition to those set forth herein. For example, the implementation described can be directed to various combinations and sub combinations of the disclosed features and/or combinations and sub combinations of the several further features disclosed above. In addition, the logic flows depicted in the accompanying figures and/or described herein do not necessarily require the order shown, or sequential order, to achieve desirable results. Other implementations may be within the scope of the following claims.

Claims

WE CLAIM

1. A biosurfactant composition comprising: guerbet alcohol salts ranges from 10- 20 % (wt/wt) of the biosurfactant composition; lauryl alcohol salts ranges from 15 to 25 % (wt/wt) of the biosurfactant composition; protein hydrolysate ranges from 1 to 5 % (wt/wt) of the biosurfactant composition; glycerine ranges from 1 to 5 % (wt/wt) of the biosurfactant composition; and extracts of soap nut ranges from 1 to 5 % (wt/wt) of the biosurfactant composition.

2. The biosurfactant composition as claimed in claim 1 , further comprising water ranging from 50-70% (vol/vol) of the biosurfactant composition.

3. The biosurfactant composition as claimed in claim 1, wherein the guerbet alcohol salts are selected from a group comprising guerbet alcohol ethoxylates, or derivatives thereof.

4. The biosurfactant composition as claimed in claim 1 , wherein the lauryl alcohol salts are selected from a group comprising alcohol ethoxylates or derivatives thereof.

5. The biosurfactant composition as claimed in claim 1, wherein extract of soap nut is from Sapindus mukorossi

6. The biosurfactant composition as claimed in claim 1, wherein upon homogenization provides an emulsion index in the range of 60-70%.

7. A method (100) of preparation of biosurfactant composition comprising: mixing (102) protein hydrolysate with water in a beaker to obtain an aqueous solution of protein hydrolysate; stirring (104) the aqueous solution obtained at step(102); adding (106) glycerol to the aqueous solution obtained at step(104) followed by agitation to obtain first mixture; adding (108) aqueous solution of soap nut extract to the mixture obtained at step 106 to obtain second mixture; and adding (110) guerbet alcohol salts and lauryl alcohol salts to the mixture obtained at step 108 to obtain the biosurfactant composition mixture.

8. The method (100) of preparation of biosurfactant composition as claimed in claim 7, wherein the biosurfactant composition obtained at step (110) is further made up to a desired volume and concentration by adding water.

9. The method (100) of preparation of biosurfactant composition as claimed in claim 7, wherein the guerbet alcohol salts are selected from a group comprising guerbet alcohol ethoxylates and/or derivatives thereof.

10. The method (100) of preparation of biosurfactant composition as claimed in claim 7, wherein the lauryl alcohol salts are selected from a group comprising alcohol ethoxylates and/or derivatives thereof.