Method for verifying a homogenizing valve

Abstract

A method for verifying a homogenization valve (1), comprising the steps of: preparing an emulsion having a hydrophilic phase and a lipophilic phase, the hydrophilic phase comprising, in weight percent of total weight: from 55% to 74% of demineralized water, from 10% to 20% of glycerol and from 3% to 4.2% of butylene glycol, the lipophilic phase comprising, in weight percent of total weight: from 5.1% to 5.9% of squalane, from 7.2% to 8.8% of alkyl ester of caprylic acid and from 0.665% to 0.735% of cetyl alcohol; subjecting the emulsion to a plurality of forced passages within the homogenization valve (1) from a high pressure zone (HP) to a low pressure zone (LP).

Description

TECHNICAL FIELD

[0001] The present invention relates to a method for verifying a homogenization valve.

[0002] The invention presented here is used in the food industry, in particular in the dairy industry, or in the chemical industry, the pharmaceutical industry or the cosmetics industry. The invention can also be used in the manufacturing sector where homogenization is a step of the production process. For example, consider the production of carbon-based nanostructured materials such as graphene and carbon nanotubes or the cell disintegration of yeasts, algae or microorganisms for the production of intracellular materials. BACKGROUND

[0003] Even in the varying, currently known embodiments, the homogenization plant comprises a high-pressure pump and a homogenization valve which acts on the fluid product in order to:

[0004] - break up the particles of the fluid so as to make their size uniform, reduce the average size and the variance of the distribution, in order to stabilize the product and increase its shelf life in the case of emulsions;

[0005] - in the case of pharmaceutical applications, break down the cell membranes in order to facilitate the extraction of the active ingredients;

[0006] - in the case of chemical applications and cellulose or unicellular organisms, modify the structure of the particles.

[0007] For most products, the main parameters that define the level of homogenization are the average particle size and the standard deviation.

[0008] According to the known solutions, the homogenization valve, placed downstream of the piston pump, comprises a first chamber which receives the fluid delivered by the pump at high pressure and a second chamber which can supply the outgoing homogenized fluid at low pressure. The homogenization action is obtained by forcing the fluid through a gap of reduced size obtained between the first chamber and the second chamber.

[0009] Both single-stage homogenizer structures and double-stage homogenizer structures are known.

[0010] So far, the testing of the homogenization plant before installation has included mechanical and electrical tests.

[0011] The water is recirculated in the homogenization valve, so it is not possible to verify the actual ability to reach the operating pressure designed for the valve.

[0012] DISCLOSURE OF THE INVENTION

[0013] In this context, the aim of the present invention is to propose a method for verifying a homogenization valve which overcomes the problems of the prior art cited above.

[0014] In particular, it is an object of the present application to propose a method for verifying a homogenization valve which allows verifying the effective homogenization capacity of the valve, i.e. the capacity of the valve to pulverize the particles of the fluid making them uniform in size.

[0015] It is a further object of the present application to provide a method for verifying a homogenization valve which is quick and easily performed by the operator.

[0016] The stated technical task and the prescribed objects are substantially achieved by a method for verifying a homogenization valve, comprising the steps of:

[0017] - preparing an emulsion having a hydrophilic phase and a lipophilic phase, the hydrophilic phase comprising, in weight percent on total weight: from 55% to 74% of demineralized water, from 10% to 20% of glycerol and from 3% to 4.2% of butylene glycol, the lipophilic phase comprising, in weight percent on total weight: from 5.1% to 5.9% of squalane, from 7.2% to 8.8% of alkyl ester of caprylic acid and from 0.665% to 0.735% of cetyl alcohol;

[0018] - subjecting the emulsion to a plurality of forced passages within the homogenization valve from a high pressure zone to a low pressure zone.

[0019] According to an aspect of the present application, the lipophilic phase of the emulsion further comprises, in weight percent on total weight: from 1.9% to 2.1% of stearic acid and from 4.75% to 7.2% of polyglyceryl-3-methyl glucose distearate.

[0020] According to an aspect of the present application, the lipophilic phase of the emulsion further comprises, in weight percent on total weight: from 1.9% to 2.1% of stearic acid and from 4.75% to 7.2% of distearate of triglycerol.

[0021] According to an aspect of the present application, the lipophilic phase of the emulsion further comprises, in weight percent on total weight: from 4.75% to 7.2% of distearate of triglycerol.

[0022] According to an aspect of the present application, the lipophilic phase of the emulsion further comprises, in weight percent on total weight: from 4.75% to 7.2% of polyglyceryl-3-methyl glucose distearate.

[0023] According to an aspect of the present application, the lipophilic phase of the emulsion further comprises, in weight percent on total weight: from 1.0% to 1.1% of triethanolamine.

[0024] According to an aspect of the present application, the emulsion is subjected to forced passages within the homogenization valve from 15 to 20 times.

[0025] According to an aspect of the present application, there is also provided a step of heating the emulsion at a temperature comprised between 20°C and 80°C before subjecting the emulsion to forced passages within the homogenization valve.

[0026] Brief description of the attached figures

[0027] Further features and advantages of the invention will become clearer from the indicative and therefore non-limiting description of a preferred, but not exclusive, embodiment of the method for verifying a homogenizing valve, as illustrated in the accompanying drawings, in which:

[0028] - Figure 1 A homogenization valve that can undergo the verification method according to the present invention is shown;

[0029] - Figure 2 This figure illustrates the effect of forced pass of the emulsion according to the verification method proposed in this paper compared to a regular emulsion.

[0030] - Figure 3 This is a graph illustrating the standard deviation of the emulsion proposed in this paper.

[0031] Detailed description of the preferred embodiments of the invention

[0032] The validation method developed in this paper involves first preparing an emulsion. As is known, an emulsion comprises a hydrophilic phase and a lipophilic phase.

[0033] The hydrophilic phase comprises, by weight percentage of the total weight:

[0034] - Softened water from 55% to 74%;

[0035] - Glycerin from 10% to 20%;

[0036] - Butanediol from 3% to 4.2%.

[0037] The lipophilic phase comprises, by weight percentage of the total weight:

[0038] - Squalane from 5.1% to 5.9%;

[0039] - Acrylic octanoate from 7.2% to 8.8%;

[0040] - Cetyl alcohol from 0.665% to 0.735%.

[0041] The lipophilic phase comprises, by weight percentage of the total weight:

[0042] - Squalane from 5.1% to 5.9%;

[0043] - Acrylic octanoate from 7.2% to 8.8%;

[0044] - Cetyl alcohol from 0.665% to 0.735%;

[0045] - Stearic acid from 1.9% to 2.1%;

[0046] - From 4.75% to 7.2% polyglycerol-3-methylglucose distearate. According to another embodiment, the lipophilic phase comprises, by weight percentage of total weight: - From 5.1% to 5.9% squalane;

[0047] - Acrylic octanoate from 7.2% to 8.8%;

[0048] - Cetyl alcohol from 0.665% to 0.735%;

[0049] - Stearic acid from 1.9% to 2.1%;

[0050] - Distearate of triglycerides from 4.75% to 7.2%.

[0051] According to another embodiment, the lipophilic phase comprises, by weight percentage of total weight: - squalane from 5.1% to 5.9%;

[0052] - Acrylic octanoate from 7.2% to 8.8%;

[0053] - Cetyl alcohol from 0.665% to 0.735%;

[0054] - Distearate of triglycerides from 4.75% to 7.2%.

[0055] According to another embodiment, the lipophilic phase comprises, by weight percentage of total weight: - squalane from 5.1% to 5.9%;

[0056] - Acrylic octanoate from 7.2% to 8.8%;

[0057] - Cetyl alcohol from 0.665% to 0.735%;

[0058] - Polyglycerol-3-methylglucose distearate from 4.75% to 7.2%.

[0059] According to another embodiment, the lipophilic phase comprises, by weight percentage of the total weight:

[0060] - Squalane from 5.1% to 5.9%;

[0061] - Acrylic octanoate from 7.2% to 8.8%;

[0062] - Cetyl alcohol from 0.665% to 0.735%;

[0063] - Stearic acid from 1.9% to 2.1%;

[0064] - Distearate of triglycerides ranging from 4.75% to 7.2%;

[0065] - Triethanolamine from 1.0% to 1.1%.

[0066] According to another embodiment, the lipophilic phase comprises, by weight percentage of the total weight:

[0067] - Squalane from 5.1% to 5.9%;

[0068] - Acrylic octanoate from 7.2% to 8.8%;

[0069] - Cetyl alcohol from 0.665% to 0.735%;

[0070] - Triethanolamine from 1.0% to 1.1%.

[0071] According to another embodiment, the lipophilic phase comprises, by weight percentage of the total weight:

[0072] - Squalane from 5.1% to 5.9%;

[0073] - Acrylic octanoate from 7.2% to 8.8%;

[0074] - Cetyl alcohol from 0.665% to 0.735%;

[0075] - Stearic acid from 1.9% to 2.1%;

[0076] - Polyglycerol-3-methylglucose distearate from 4.75% to 7.2%;

[0077] - Triethanolamine from 1.0% to 1.1%.

[0078] Once prepared, the emulsion is in the process of... Figure 1 The number 1 indicates that the homogenizing valve is forced to pass from the high-pressure zone HP to the low-pressure zone LP.

[0079] Specifically, the emulsion is forced through the homogenizing valve 1 multiple times.

[0080] Such forced passage can be performed in a recirculation or through a separate channel. A stop can also be set between one channel and another.

[0081] The number of times it passes depends on the specific verification.

[0082] According to the implementation scheme of this method, the forced passage in the homogenizing valve 1 occurs from 15 to 20 times.

[0083] According to an aspect of the invention, the emulsion is heated to a temperature between 20°C and 80°C before forced passage.

[0084] All of the above emulsion formulations have been used to validate a two-stage homogenization device, which has a heat exchanger and operates at a maximum pressure of 1000 bar.

[0085] The results show that the emulsion becomes increasingly transparent and translucent as the number of forced passes through the homogenizing valve increases. This allows for immediate assessment of the homogenizing effect of the device (i.e., the valve).

[0086] This validation method can be used for any homogenizing valve. The only difference lies in the amount of emulsion required to implement the method, which varies depending on the type of valve.

[0087] In the various emulsion compositions indicated above, the following allows for good particle reduction: the hydrophilic phase is always the same, while the lipophilic phase is contained, in weight percentage of the total weight:

[0088] - Squalane from 5.1% to 5.9%;

[0089] - Acrylic octanoate from 7.2% to 8.8%;

[0090] - Cetyl alcohol from 0.665% to 0.735%;

[0091] - Stearic acid from 1.9% to 2.1%;

[0092] - Distearate of triglycerides from 4.75% to 7.2%.

[0093] Among the various emulsion compositions indicated above, the following are emulsion compositions that allow for a more significant reduction in particle size and have a lower viscosity compared to other variants: the hydrophilic phase is always the same, while the lipophilic phase is contained, in weight percentage of the total weight:

[0094] - Squalane from 5.1% to 5.9%;

[0095] - Acrylic octanoate from 7.2% to 8.8%;

[0096] - Cetyl alcohol from 0.665% to 0.735%;

[0097] - Stearic acid from 1.9% to 2.1%;

[0098] - Polyglycerol-3-methylglucose distearate from 4.75% to 7.2%;

[0099] - Triethanolamine from 1.0% to 1.1%.

[0100] This emulsion composition is considered optimal compared to all other emulsion compositions.

[0101] The conceived emulsion, in its various implementations, allows for efficient homogenization over a wider operating range compared to "general" emulsions.

[0102] This property is illustrated by the curves shown in the graph. Figure 2 As shown in the figure, the horizontal axis indicates the number of times the material is forced through the homogenizing valve, and the vertical axis indicates the particle size in nm.

[0103] The curves associated with typical emulsions are solid lines. Such emulsions contain water (80.5%), sunflower oil (15%), and a combination of two surfactants: Tween 80 (2.45% of a surfactant with formula C...). 64 H 124 O 26 Polysorbate 80 and commercially available surfactants SMO80 (2.05%).

[0104] The emulsion-related curves presented here are dashed lines. The selected emulsion composition is the optimal emulsion composition identified above.

[0105] Comparing the two curves, we can notice that:

[0106] - Under the same number of passes in the same homogenizing valve, the designed emulsion results in a larger particle size reduction than that of a typical emulsion;

[0107] - The designed emulsion allows for achieving the desired final particle size with fewer passes.

[0108] The envisioned emulsion allows for visual assessment of quality and homogenization in relation to the operating conditions used.

[0109] Given the wide working area, the conceived emulsion allows for better differentiation of two close working points in terms of particle size (in this example, it ranges from 80 nm to 160 nm) compared to a typical emulsion.

[0110] For the preparation of the emulsion presented here, some commercial products can be used, such as:

[0111] - Care 450 (polyglycerol-3-methylglucose distearate);

[0112] - GS 32 (distearate of triethylene glycol).

[0113] Based on the provided description, the features and advantages of the method for verifying a homogenizing valve according to the present invention are clear.

[0114] In particular, the proposed verification method allows for the verification of the valve's actual homogenization capability. This is not merely a mechanical and / or electrical function test, but also a test simulating real-world operating conditions, as the parameters of the homogenized emulsion are evaluated.

[0115] Therefore, homogenizers that meet high-quality standards and have higher reliability are manufactured for use by end users.

[0116] The specific composition of the emulsion (and its variants) presented here allows for the development of a universal validation method that can be used with any type of homogenizing valve. In fact, it is sufficient to vary the amount of emulsion according to the characteristics of the homogenizing valve.

[0117] Furthermore, the verification method presented here is complete and reliable, meaning it does not require confirmation from other tests.

[0118] Furthermore, since effectively homogenized emulsions are transparent, stable, and translucent, the homogenization effect is quickly and easily verified by the operator's naked eye.

[0119] Furthermore, compared to other emulsions on the market, the emulsion presented here results in a smaller particle size (with significant energy savings) through fewer passes, or smaller particle size through the same number of passes.

[0120] The proposed verification method is reliable and cost-effective because it is based on a stable, low-viscosity, and low-cost emulsion.

Claims

1. A method for verifying a homogenization valve (1), comprising the steps of: preparing an emulsion having a hydrophilic phase and a lipophilic phase, said hydrophilic phase comprising, in weight percent of total weight: from 55% to 74% of demineralized water, from 10% to 20% of glycerol and from 3% to 4.2% of butylene glycol, said lipophilic phase comprising, in weight percent of total weight: from 5.1% to 5.9% of squalane, from 7.2% to 8.8% of alkyl ester of caprylic acid and from 0.665% to 0.735% of cetyl alcohol; subjecting said emulsion to from 15 to 20 forced passes within said homogenization valve (1) from a high pressure zone (HP) to a low pressure zone (LP).

2. The method according to claim 1, wherein said lipophilic phase of said emulsion further comprises, in weight percent of total weight: from 1.9% to 2.1% of stearic acid and from 4.75% to 7.2% of polyglyceryl-3-methylglucose distearate.

3. The method according to claim 1, wherein said lipophilic phase of said emulsion further comprises, in weight percent of total weight: from 1.9% to 2.1% of stearic acid and from 4.75% to 7.2% of distearate of triglycerol.

4. The method according to claim 1, wherein said lipophilic phase of said emulsion further comprises, in weight percent of total weight: from 4.75% to 7.2% of distearate of triglycerol.

5. The method according to claim 1, wherein said lipophilic phase of said emulsion further comprises, in weight percent of total weight: from 4.75% to 7.2% of polyglyceryl-3-methylglucose distearate.

6. The method according to any one of the preceding claims, wherein said lipophilic phase of said emulsion further comprises, in weight percent of total weight: from 1.0% to 1.1% of triethanolamine.

7. The method according to any one of the preceding claims, further comprising the step of heating said emulsion at a temperature comprised between 20°C and 80°C, before subjecting said emulsion to forced passes within said homogenization valve (1).

8. Use of an emulsion for verifying a homogenization valve (1), said emulsion having a hydrophilic phase and a lipophilic phase, said hydrophilic phase comprising, in weight percent of total weight: from 55% to 74% of demineralized water, from 10% to 20% of glycerol and from 3% to 4.2% of butylene glycol, said lipophilic phase comprising, in weight percent of total weight: from 5.1% to 5.9% of squalane, from 7.2% to 8.8% of alkyl ester of caprylic acid and from 0.665% to 0.735% of cetyl alcohol.

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