Clarification reagent

Abstract

The use of porous colloidal or precipitated silica particles in the treatment of wort is described, wherein the porous silica particles have a water content of 30% by weight or less and a pore volume of 0.4 ml / g or greater. Methods of treating wort and methods of making a beverage are also described.

Description

Technical Field

[0001] This invention relates to the use of porous silica particles in wort treatment, methods for wort treatment, and methods for preparing liquid beverages. Background Technology

[0002] It is well known that the brewing process typically produces beverages with high levels of haze, such as beer. For some end-consumer products, this haze may be undesirable, where consumers may require clarification of the product.

[0003] In a typical method, the beverage obtainable from wort (e.g., beer) is clarified in a cold block after fermentation by treatment with colloidal stabilizer agents. These agents are then removed from the final product by filtration. Various clarifying agents have been used in the art for this post-production clarification, and silica hydrogels are known, for example, for this purpose. Although less frequently used, brewers also know to add refining agents to the wort prior to fermentation. These agents have the effect of coagulating coarse particles and / or removing at least some turbidity from the wort. Exemplary refining agents include carrageenan, tannic acid, polyvinylpyrrolidone (PVPP), gelatin, fish glue, egg white, casein, bentonite, and carbon. Mixtures of materials, such as carrageenan and PVPP (e.g., Polyclar, manufactured by Ashland Global Specialty Chemicals Inc.), are also used. TM Carrageenan and silica sol (e.g., GB2280908A), carrageenan and carbohydrates (e.g., US6045852A), or combinations of silica hydrogels and PVPP (e.g., PolyGel BH provided by AEB group). The independent use of silica sol as a refining agent is also known, for example, in US8697169B2. Silica sol is essentially a stable aqueous suspension of colloidal, non-porous silica particles.

[0004] However, the above strategy has several drawbacks, such as insufficient clarification and / or the need for additional processing steps and / or reduced efficiency of the overall process. For example, not all breweries have space for cold block filtration, and furthermore, filtration to remove fine particles can often reduce efficiency, such as due to filter clogging / increased back pressure on the filter, which can reduce production volume.

[0005] Producers of non-fermented beverages that can be obtained from wort also encounter the above problems, among which more clarified products are desired.

[0006] Therefore, it would be beneficial to have alternative and / or improved methods for producing beverages with the desired level of clarity that can be obtained from wort. Summary of the Invention

[0007] At a general level, this invention presents novel uses of specific porous silica particles for wort treatment, offering surprising advantages. In particular, it has been found that the use of porous silica sol particles or porous precipitated silica particles as described herein can reduce wort turbidity and, in some embodiments, also reduce the protein content of the wort. The use of these silica particles has been found to provide significant advantages over prior art methods (such as those described above), for example, compared to the use of silica sol.

[0008] Advantageously, it has been found that using the silica particles described herein provides a significant reduction in wort turbidity at relatively low loading levels (see Examples).

[0009] Advantageously, it has also been found that some embodiments of the invention reduce the amount of sensitive proteins present. It should be understood that the term "sensitive protein" refers to a protein fraction that can be precipitated by tannins. Therefore, as described in the Method section below, the amount of sensitive protein is determined by measuring the turbidity (EBC units) formed after the addition of a specific amount of tannins. Reduction of sensitive proteins allows breweries to reduce or avoid the need for post-fermentation beer stabilization. This is particularly advantageous for smaller breweries that do not have the possibility of stabilization and filtration in cold blocks, or for breweries that want to avoid process bottlenecks later in the process, which can reduce the yield of the final product.

[0010] The reduction in turbidity and protein content also offers further advantages. Wheat treated with silica particles according to the invention has shown the potential to spend less time in the whirlpool stage of the process, while producing a more compact thermal trub, resulting in increased yield.

[0011] Furthermore, it has been unexpectedly observed that using the method according to the invention results in improvements in the subsequent filtration of fermented beer obtained from the treated wort. For example, the use of porous silica particles in the brewing process described herein has been shown to result in less charge entering the filter, and therefore less pressure buildup on the filter during longer filtration runs. For example, as described below, it has been found that approximately twice the volume of beer can be filtered in the same run compared to beer fermented from wort that has never been treated with the porous silica particles of the invention.

[0012] Therefore, it has been found that using the silica particles described herein provides a high level of turbidity reduction and, in some embodiments, a high level of sensitive protein removal, even when used in low doses, while also delivering practical benefits in terms of processability. Thus, the use of the silica particles described herein can improve the overall efficiency of the brewing process.

[0013] Furthermore, this method provides reduced waste compared to conventional brewing methods that involve post-fermentation clarification. For example, the silica particles used can be separated from the waste grains of the wort and used in animal feed or sent to a methanation (biogas) plant. Conventional methods involving clarification in cold blocks generate separate waste products.

[0014] In a first aspect of the invention, the use of porous silica granules or porous precipitated silica particles in the treatment of wort is provided, wherein the porous silica particles have a water content of 30% by weight or less and a pore volume of 0.4 ml / g or greater. It should be understood herein that "porous silica particles" refers to both the aforementioned porous silica granules and porous precipitated silica particles.

[0015] The term "wort" is well-known in the art and is intended to be used in its conventional sense. This term includes, for example, the liquid extracted from grains obtained during the saccharification step of the brewing process. Examples include wort obtained from brewing beers such as larger lagers, pilsners, Dortmund beers, and Munich beers, as well as top-fermented beverages such as ale, porter, and stout. Wort typically contains proteins in addition to sugars (such as maltose), which will (in the case of fermented products) be fermented by yeast to produce fermented beverages. Wort can be, for example, a whole-malt brew or a partially malted brew with adjuncts, such as 60% malt and 40% adjuncts.

[0016] The term "moisture content" for grains refers to the moisture content of the grains before the addition of wort in the process. Moisture content can be calculated using the methods described below in the General Methods section for "Determining Moisture Content".

[0017] As described above, this method has advantageously demonstrated a significant reduction in turbidity levels, and in some embodiments, a significant reduction in protein levels. This reduction eliminates the need for further post-fermentation processing and improves the efficiency of the vortex and filtration stages of the brewing process, resulting in a more optimized brewing process.

[0018] In a second aspect of the invention, a method for treating wort is provided, comprising contacting the wort with porous silica particles or porous precipitated silica particles, wherein the porous silica particles have a water content of 30% by weight or less and a pore volume of 0.4 ml / g or greater. It should be understood herein that "porous silica particles" refers to both the aforementioned porous silica particles and porous precipitated silica particles.

[0019] In a third aspect of the invention, a method for preparing a beverage is provided, comprising: treating grains to produce wort; contacting the wort with porous silica particles or porous precipitated silica particles; and using the resulting wort to produce a beverage; wherein the porous silica particles have a water content of 30% by weight or less and a pore volume of 0.4 ml / g or greater. It should be understood herein that "porous silica particles" refers to both the aforementioned porous silica particles and porous precipitated silica particles.

[0020] As will be understood based on the advantages described herein (and demonstrated by examples), the wort treatment according to the uses and methods of the invention has the effect of reducing wort turbidity (based on the turbidity value determined by the methods described herein), and in embodiments may also reduce the protein level in the wort, particularly the level of sensitive proteins (also as further described herein). Therefore, in the uses and methods described herein, wort treatment may be for the purpose of reducing wort turbidity and optionally reducing the protein content of the wort.

[0021] Therefore, the use of porous silica granules or porous precipitated silica particles in reducing wort turbidity (and optionally, the protein content of wort) is provided, wherein the porous silica particles have a water content of 30% by weight or less and a pore volume of 0.4 ml / g or greater. It should be understood herein that “porous silica particles” refers to both the porous silica granules and porous precipitated silica particles mentioned herein.

[0022] A method for reducing wort turbidity (and optionally, the protein content of the wort) is also provided, comprising contacting the wort with porous silica particles or porous precipitated silica particles, wherein the porous silica particles have a water content of 30% by weight or less and a pore volume of 0.4 ml / g or greater. It should be understood herein that “porous silica particles” refers to both the aforementioned porous silica particles and porous precipitated silica particles.

[0023] It should also be understood that in the method of preparing a beverage provided as in the third aspect and embodiments of the present invention, contacting wort with porous silica particles or porous precipitated silica particles has the effect of reducing wort turbidity (the turbidity value determined according to the method described herein), and in embodiments, it can also reduce the protein level in the wort, particularly the level of sensitive proteins (also as further described herein). Therefore, a method of preparing a beverage is also provided, comprising: treating grains to produce wort; contacting the wort with porous silica particles or porous precipitated silica particles to reduce the turbidity of the wort (and optionally also reduce the protein content of the wort); and using the resulting wort to produce a beverage; wherein the porous silica particles have a water content of 30% by weight or less and a pore volume of 0.4 ml / g or greater. It should be understood herein that “porous silica particles” refers to the aforementioned porous silica particles and porous precipitated silica particles. Detailed Implementation

[0024] Embodiments of various aspects of the present invention are described below. To avoid ambiguity, it should be understood that any embodiment described herein with respect to one aspect of the invention will also apply to other aspects of the invention where appropriate.

[0025] Unless otherwise stated herein, the nature attributed to "porous silica particles" in the statements and claims of this invention refers to both the porous silica gel particles and the porous precipitated silica particles mentioned herein.

[0026] According to the present invention, porous silica particles (i.e., porous silica granular particles and porous precipitated silica particles) may have a pore volume of 0.6 ml / g or greater, such as 0.75 ml / g or greater, or 0.8 ml / g or greater. Porous silica particles may also have a pore volume of 2 ml / g or less. Therefore, porous silica particles (i.e., porous silica granular particles and porous precipitated silica particles) may have a pore volume from 0.6 ml / g to 2 ml / g.

[0027] Porous silica particles (i.e., porous silica granular particles and porous precipitated silica particles) can have a pore volume of 1.0 ml / g or greater. For example, porous silica particles can have a pore volume of 1 ml / g to 2 ml / g. Porous silica particles can have a pore volume of 1.8 ml / g or less. Therefore, porous silica particles (i.e., porous silica granular particles and porous precipitated silica particles) can have a pore volume of 1 ml / g to 1.8 ml / g. Porous silica particles can have a pore volume of 1.0 ml / g to 1.2 ml / g.

[0028] As illustrated in the following examples, increasing the pore volume has been observed to affect the achievable reduction in turbidity and the reduction in sensitive protein levels. As shown in Tables 2 and 5, pore volumes above 1.0 ml / g exhibited improvements over test examples with pore volumes below that value. Particularly favorable results were obtained using pore volumes between 1.0 and 1.8 ml / g, where the test examples showed particularly significant improvements in both turbidity and sensitive protein reduction compared to relatively low or high pore volumes.

[0029] Porous silica particles (i.e., porous silica gel particles and porous precipitated silica particles) may have a pore volume of 1.2 ml / g or greater. Porous silica particles may have a pore volume of 1.2 ml / g to 2 ml / g. Porous silica particles may have a pore volume of 1.2 ml / g to 1.8 ml / g. Porous silica particles may have a pore volume of 1.2 ml / g to 1.3 ml / g, for example, about 1.28 ml / g. Porous silica particles may have a pore volume of 1.5 ml / g or greater, for example, porous silica particles may have a pore volume of 1.5 ml / g to 2 ml / g. Porous silica particles may advantageously have a pore volume of 1.5 ml / g to 1.8 ml / g. The aforementioned porous silica particles may have a pore volume of 1.6 ml / g or greater. Porous silica particles can have a pore volume of 1.6 ml / g to 1.8 ml / g, for example, about 1.7 ml / g.

[0030] In some embodiments, the porous silica particles may have a pore volume of 1.75 ml / g or greater, such as 1.8 ml / g or greater. In other embodiments, the porous silica particles have a pore volume of 1.75 ml / g or less, such as 1.6 ml / g or less, such as 1.5 ml / g or less. Optionally, the lower end of these ranges may be a pore volume of 1.0 ml / g.

[0031] Porous silica particles (i.e., porous silica gel particles and porous precipitated silica particles) may have a water content of 20% by weight or less. Porous silica particles may have a water content of 15% by weight or less, for example, 10% by weight or less. Porous silica particles may have a water content of 7.5% by weight or less. Porous silica particles may have a water content of 5% by weight or less. Porous silica particles may have a water content of 1% to 10% by weight. Porous silica particles may have a water content of 2% to 6% by weight. Porous silica particles may have a water content of 2% to 4% by weight.

[0032] As described above, and as shown in Table 1, it has been found that using silica particles with a water content of less than 30% provides greater clarity compared to using the same dosage of silica particles with a higher water content. It has also been found that using silica particles with a low water content provides improvements in overall processing efficiency and ease of handling.

[0033] Advantageously, the porous silica particles of the present invention described herein provide excellent results without the need for additional refining reagents. Therefore, in embodiments, the silica particles can be used in the absence of other refining / clarifying reagents (in the methods and uses described herein), for example, in the absence of polyvinylpyrrolidone (PVPP), and / or in the absence of carrageenan or tannic acid.

[0034] As described herein, the uses and methods of the present invention may utilize porous silica granules or porous precipitated silica particles with a water content of 30% by weight or less and a pore volume of 0.4 ml / g or greater. Both porous silica granules and porous precipitated silica particles may be present, or only porous silica granules may be present, or only porous precipitated silica particles may be present. The porous silica particles can therefore be porous silica granules. For example, the porous silica particles may be porous silica degel particles. Alternatively, the porous silica particles may be porous precipitated silica particles. Both types of particles have shown particular effectiveness in reducing wort turbidity, as demonstrated in the examples below.

[0035] Porous silica particles (i.e., porous silica gel particles and porous precipitated silica particles) can have a diameter of 800 μm. 2 / g or less, such as 700 m 2 / g or less, or 600 m 2 / g or smaller surface area. The surface area of ​​porous silica particles can be 500 m². 2 / g or less, for example 450 m 2 / g or smaller. Porous silica particles can have a density of 200 μm. 2 / g or greater surface area. Therefore, porous silica particles can have a surface area of ​​200 m². 2 / g to 800 m 2 / g surface area. Preferably, the porous silica particles have a surface area of ​​200 μm. 2 / g to 500 m 2 / g of surface area.

[0036] Porous silica particles can be used in amounts from 1 g to 50 g per 100 liters of wort, such as 5 g to 20 g, or 10 g to 30 g per 100 liters of wort. Porous silica particles can also be used in amounts not exceeding 25 g per 100 liters of wort, for example, about 20 g per 100 liters of wort. Advantageously, it has been found that the silica particles described herein provide a significant reduction in wort turbidity even at relatively low loadings, resulting in excellent efficiency (see Table 4 in the examples below). The ability to use lower silica content to achieve desired turbidity and / or protein levels is also expected to lead to downstream processing benefits, as less fines (finings) material must then be removed from the product. Therefore, porous silica particles can be used in amounts not exceeding 20 g per 100 liters of wort. Porous silica particles can also be used in amounts not exceeding 15 g per 100 liters of wort, not exceeding 10 g per 100 liters of wort, or not exceeding 8 g per 100 liters of wort. Porous silica particles can be used in amounts of 1 g to 15 g per 100 liters of wort, such as 1 g to 10 g, 1 g to 8 g, or 1 g to 5 g per 100 liters of wort.

[0037] Porous silica particles can have a median weight particle size (D50) of 1 μm or greater. Porous silica particles can have a median weight particle size (D50) of 2.5 μm or greater. Porous silica particles can have a median weight particle size (D50) of 5 μm or greater, such as 7.5 μm or greater, or 10 μm or greater. Advantageously, the use of micron-sized particles allows silica particles to settle more easily from the solution and thus be removed from the wort after processing. This represents an improvement over colloidal silica.

[0038] Porous silica particles may have a median weight particle size (D50) of 200 μm or less. Porous silica particles may have a median weight particle size (D50) of 150 μm or less, 100 μm or less, 80 μm or less, or 50 μm or less. The median weight particle size (D50) of the porous silica particles is less than 30 μm. Porous silica particles have a median weight particle size (D50) of 20 μm or less, for example, 15 μm or less. Therefore, porous silica particles may have a median weight particle size (D50) from 1 μm to 200 μm. Preferably, porous silica particles have a median weight particle size (D50) from 2.5 μm to 80 μm. Porous silica particles may have a median weight particle size (D50) from 5 μm to 50 μm. As shown in Table 5, silica particles with higher median weight size (D50), particularly those above 80 μm, were found to show less reduction in sensitive proteins compared to silica particles with lower median weight size (D50).

[0039] In a preferred embodiment, the porous silica particles have a pore volume of 1.2 ml / g to 1.3 ml / g, a water content of 2% wt to 4% wt, and a median particle size (D50) of 5 μm to 50 μm. The porous silica particles of this preferred embodiment may be porous silica xerogel particles.

[0040] In another preferred embodiment, the porous silica particles have a pore volume of 1.0 ml / g to 1.2 ml / g, a water content of 2% to 6%, and a median weight particle size (D50) of 2.5 μm to 50 μm. The porous silica particles in this preferred embodiment may be precipitated silica particles.

[0041] In another preferred embodiment, the porous silica particles have a pore volume of 1.6 ml / g to 1.8 ml / g, a water content of 2% to 4%, and a median weight particle size (D50) of 5 μm to 50 μm. The porous silica particles in this preferred embodiment may be porous silica gel particles, such as silica desiccant particles.

[0042] According to the present invention, the wort can be treated at any suitable point in the beverage preparation process. It should be understood that the method is not particularly limited by the location of the wort. For example, contacting porous silica particles with the wort can occur in a mashing tank, a filter tank, a filter press, a wort pot, a vortex / decanter, or a fermentation tank, or any two of the above. It can also occur in different locations.

[0043] The uses and methods described herein may also include precipitating silica particles from the wort and separating the wort from the silica particles. This allows for the easy removal of silica particles and any adsorbed compounds from the wort.

[0044] The uses and methods described herein may further include treating grains to produce wort, subsequently contacting the wort with porous silica particles or porous precipitated silica particles. The method may further include using the resulting wort (i.e., after treatment with porous silica particles) to produce a beverage. Therefore, the method may further include treating grains to produce wort and using the resulting (treated) wort to produce a beverage.

[0045] Therefore, a method according to a third aspect of the invention is provided.

[0046] The method according to the third aspect or its embodiments may also include separating silica particles from the wort before using the resulting wort to produce a beverage. Separating the particles at this stage can improve downstream processing, such as pressure on filter elements.

[0047] Silica particles can be separated from wort along with waste grains generated from grain processing. Advantageously, this avoids the need for a separate waste stream, allows the particles to be used or processed together with the waste grains, and improves the efficiency of the clarification process.

[0048] Preferably, the method is a method for brewing a fermented beverage, and the wort used includes fermented wort. In other words, a method for brewing a fermented beverage is provided, comprising: processing grains to produce wort; contacting the wort with porous silica particles or porous precipitated silica particles; and fermenting the wort to produce a fermented beverage; wherein the porous silica particles have a water content of 30% by weight or less and a pore volume of 0.4 ml / g or greater.

[0049] In a particularly preferred embodiment, the fermented beverage is beer.

[0050] In some embodiments, the methods or uses described herein result in a turbidity reduction of at least 20% relative to the turbidity of the wort prior to treatment / contact with the porous silica particles of the present invention. Turbidity may be reduced by at least 25%. Turbidity may be reduced by at least 30%. Turbidity may be reduced by at least 35%. Turbidity may be reduced by at least 40%. Turbidity may be reduced by at least 45%. Turbidity may be reduced by at least 50%. Turbidity may be reduced by at least 55%. Turbidity may be reduced by at least 60%. Turbidity may be reduced by at least 65%. Turbidity may be reduced by at least 70%. Turbidity may be reduced by at least 75%. Turbidity may be reduced by at least 80%. Turbidity may be reduced by at least 85%. Turbidity may be reduced by at least 90%. Turbidity may be reduced, for example, by 20-90% or 20-50%. The reduction in turbidity is determined according to the methods described herein for determining the level of turbidity reduction (see the General Methods section).

[0051] In some embodiments, the methods or uses described herein result in a reduction of sensitive protein content of at least 5% relative to the sensitive protein content of the wort prior to treatment / contact with the porous silica particles of the present invention. A reduction of at least 10% may be present. A reduction of at least 15% may be present. A reduction of at least 20% may be present. A reduction of at least 25% may be present. A reduction of at least 30% may be present. A reduction of at least 35% may be present. A reduction of at least 40% may be present. A reduction of at least 45% may be present. For example, sensitive protein may be reduced by 5-45%. The reduction in sensitive protein is determined according to the methods described herein for determining the level of sensitive protein reduction (see the General Methods section). Attached Figure Description

[0052] Figure 1 This is a graph showing the turbidity levels in wort samples after laboratory-scale treatment with different silica gels.

[0053] Figure 2This is a graph showing the reduction in protein in wort samples after laboratory-scale treatment with low-water-content silica gels of different pore volumes.

[0054] General methods

[0055] Determining water content

[0056] The water content of silica particles is determined by measuring the weight loss after drying at 105°C and atmospheric pressure (e.g., using an oven) for 4 hours. This method is the standard method for measuring the water content of silica.

[0057] Determine turbidity level

[0058] The turbidity of the wort sample was measured at room temperature using a turbidimeter (Hach 2100N) and expressed in EBC 90° turbidity units. This refers to the EBC units measured in the turbidimeter at a 90-degree angle.

[0059] The turbidity reduction was calculated by comparing the turbidity value (EBC 90° turbidity units) of the wort sample treated with silica particles with that of a reference sample not treated with silica particles. The turbidity value of the wort sample treated with silica particles was recorded 20 minutes after contact with the wort. Simultaneously (also after 20 minutes), the turbidity value of the reference sample was recorded. The following formula was used for calculation.

[0060]

[0061] In each table, a reference sample is provided as a comparison example for the calculation.

[0062] Determining the amount of sensitive proteins

[0063] The presence of sensitive proteins in beverages derived from wort (e.g., beer) can adversely affect beverage stability. The effect of the porous silica clarifying agent of the present invention on reducing sensitive proteins was tested. As mentioned above, the amount of sensitive proteins referred to herein refers to the portion of proteins that are precipitable by tannins. More information can be found in KALeiper et al., Optimisin g Beer Stabilisation by the Selective Removal of Tannoids and Sensitive Proteins”, Journal of the Institute of Brewing g, 111(2), 118-127, 2005.

[0064] Sensitive proteins were determined using the method described in European Brewery Convention (EBC) Analytica, Section 9.40, Sensitive proteins in beer by nephelometry, Fachverla g Hans Carl, Nürenber g, Germany, 1998. This method was modified by performing measurements after 30 minutes. In short, after performing the turbidity measurement protocol (as described above), the turbidity value was remeasured, and a 0.1 g / L aqueous solution of tannic acid was added to both the wort sample treated with silica particles and the corresponding reference sample. The amount of precipitated “sensitive proteins” was then measured as the increase in wort turbidity at a predetermined time (30 minutes) after the addition of tannic acid. In this specific case, 20 ml of the 0.1 g / L tannic acid solution was added to 180 ml of wort (with stirring). Sensitive proteins are expressed in EBC 90° turbidity units (turbidimeter (Hach 2100N)).

[0065] The reduction in sensitive proteins is calculated by comparing the sensitive protein values ​​of wort samples treated with silica particles with those of a reference sample not treated with silica particles. The following formula is used for calculation:

[0066]

[0067] In each table, a reference sample is provided as a comparison example for the calculation.

[0068] Surface area and pore volume measurement

[0069] The surface area of ​​silica was determined using the standard multipoint nitrogen adsorption method of Brunauer, Emmett, and Teller (BET) with an ASAP 2460 apparatus provided by Micromeritics, USA. This method is consistent with the paper by S. Brunauer, PHEmmett, and E. Teller (J. Chem. Soc., 60, 309 (1938)).

[0070] The silica pore volume was determined using the same instrumentation as described in ASTM D4222-20. The total pore volume was measured from the desorption branch of the isotherm at a partial pressure P / P0 of 0.998.

[0071] The dry gel and precipitated silica samples were degassed under vacuum at 270°C for 4 hours, and then their surface area or pore volume was measured at approximately -196°C. The hydrogel and hydrated dry gel samples were first degassed at 90°C for 1 hour, and then at 270°C for 4 hours.

[0072] Determine the aperture

[0073] The aperture is a calculated parameter based on the assumption of a cylindrical aperture. It is determined using the following equation:

[0074]

[0075] The pore volume and surface area were determined using the methods described above.

[0076] Particle size determination

[0077] The weight median particle size (D(50)) of silica particles was determined by laser diffraction using a Malvern Mastersizer 3000 and a HydroLV dispersion unit. Mie theory was used to calculate the particle size distribution. The real part of the refractive index of silica was assigned a value of 1.46, and the imaginary part of the refractive index of the particles was assigned a value of 1.0, with the real part of the refractive index of the aqueous dispersant being 1.33. Silica particles were ultrasonically dispersed in deionized water at 50% power for 2 minutes to form an aqueous suspension using a Hydro LV dispersion unit. The intensity of scattered light was measured as a function of angle, and the data were used to calculate the particle size distribution.

[0078] Laboratory-scale treatment of wort using porous silica particles

[0079] The wort samples were obtained during the transfer from the wort tank to the vortex (i.e., after the wort boiled).

[0080] Silica particles were added to the hot wort at a predetermined dose (20 g silica / 100 L wort, unless otherwise specified). The typical temperature of the hot wort can be between 70°C and 120°C, depending on the specific brewing process. In the embodiments described herein, the wort samples were obtained at approximately 100°C at the time of sampling, and the silica particles were added to the wort samples within approximately 5 minutes of sampling. Silica can be appropriately added to the wort directly or via a metering container. The wort / silica mixture was mixed with a motion similar to that of a brewery vortex. Turbidity measurements (EBC 90°) were performed using the above procedure after a predetermined time period (20 minutes after silica addition, as shown in the table below). Protein measurements were performed 30 minutes after the addition of tannins, as described in the Method section above. The wort tested in the embodiments was obtained from the following malts / brews:

[0081] 1. Whole malt, 16°P, brewed;

[0082] 2.15-16°P whole malt brews;

[0083] 3.60% malt and 40% adjunct brewing, at 18-18.5 °P.

[0084] As those skilled in the art will understand, the unit °P refers to "Pareto degree," a conventional term used to quantify the concentration of extracts (primarily sugars) in wort as a weight percentage. For example, 10°P wort would contain 10 g of extract per 100 g of wort. Information regarding the °P value of the malt is calculated using conventional methods and provided by the respective brewer. A dosage of 20 g / hl (0.2 g / l) is chosen as the corresponding dosage for conventional refining.

[0085] Industrial-scale processing of wort using porous silica particles

[0086] The use of porous silica particles during beer production was tested on a larger scale (see Example 33) to observe overall processing benefits. The beer was a 60% malt and 40% adjunct brew, 18–18.5 °P (wort 3 above). Using a hop container as the metering point, silica particles were added to the wort in the wort pot at the start of boiling. A reference brew was also prepared without adding silica particles to the wort.

[0087] Example

[0088] Various aspects of the invention will now be further described with reference to the accompanying drawings and various non-limiting embodiments.

[0089] Turbidity measurement of wort after treatment with silica particles with different water contents (Examples 1-6)

[0090] Wort samples were obtained from three different brews during the transfer from the wort tank to vortex settling. The wort was from a whole malt 16°P brew (wort 1 above). Each sample was then divided into five subsamples. One subsample of each wort sample (comparative examples C1, C4, and C7) was measured without the addition of silica particles. The remaining four samples were treated with different silica particles (broadly described as silica hydrogels, hydrated silica degels, silica degels, and high-porosity silica degels) at a concentration of 20 g / hl, as described in more detail in the examples, as described in the General Methods section above. The results are shown in Table 1 and plotted on [the table]. Figure 1 middle.

[0091] Many types of silica that can be used in the applications described herein are known in the art. Suitable silica gels can be broadly classified into two groups: hydrogels and desiccants. Partial drying of hydrogels can produce a third type, which is referred to below as “hydrated desiccants.” All three gel types can be produced according to conventional methods, such as those described in numerous publications, including, but not limited to, U.S. Patent Nos. 4,515,821, 4,636,394, 5,622,743, 6,555,151, 6,565,905, and 10,633,621, the entire subject of which is incorporated herein by reference. Methods for preparing suitable precipitated silica are described in EP0287232 and elsewhere.

[0092] The specific physical properties of each tested silica particle are presented in the table below. Comparative examples C2-3, C5-6, and C8-9 are silica particles (hydrogels and hydrated degels) with a water content of more than 30 wt%.

[0093] Table 1

[0094]

[0095] As can be seen, compared with the corresponding comparative examples, at a dosage concentration of 20 g reagent / 100 L wort (conventional refining dose), the turbidity of Examples 1-6 was significantly reduced.

[0096] Turbidity and sensitive protein levels were reduced by using low-water-content silica particles with different pore volumes (Examples 7-21).

[0097] As described above, wort samples were obtained during the transfer from the wort tank to vortex settling. The wort was wort 1 as described above. The wort was then treated with a series of low-water-content silica particles at a concentration of 20 g / hl. The silica particles tested included degelatinized and precipitated silica. The reduction in turbidity after 20 minutes and the reduction in sensitive protein content after 30 minutes were measured as described in the Methods section above. The results are shown in Table 2.

[0098]

[0099] Table 2

[0100] As can be seen from the above data, the silica particles according to the present invention exhibit a significant reduction in turbidity compared to untreated wort. It is also evident that the higher pore volume of the silica of the present invention, compared to the lower pore volume, shows improved protein reduction. For example, Examples 10-12 with a pore volume of 1.72 ml / g showed at least a 27% protein reduction, while Examples 15-17 with a pore volume of 0.51 ml / g showed a maximum reduction of 4%. This is... Figure 2The figure is presented graphically, showing the correlation between pore volume and the reduction of sensitive proteins.

[0101] Turbidity of wort was reduced after treatment with various silica dry gels (Examples 22-30)

[0102] As described above, samples from two different worts were obtained during the transfer from the wort tank to vortex settling. The first wort was a pure malt beer at 15-16°P (wort 2 above). The second wort was 60% malt and 40% adjuncts (18-18.5°P) (wort 3 above). Each wort was then treated with different silica dry gel particles (dry gel 12 to 15) at a concentration of 20 g / hl. Turbidity levels were measured after 20 minutes as described in the Methods section above. The volume of the thermally coagulated material was also measured after 20 minutes. The results are shown in Table 3.

[0103]

[0104] Table 3

[0105] As demonstrated above, the use of silica particles is suitable for both pure malt and mixed malt. In all cases, a significant reduction in turbidity and a more compact thermal solidify are achieved.

[0106] Dosage levels (Examples 28-30)

[0107] Experiments were conducted to confirm the effect of silica particle dosage relative to wort dosage on turbidity reduction. As described above, wort samples were obtained during transfer from the wort tank to vortex settling. The wort was a brewed product of pure malt beer at 15–16°P (wort 2 above). Silica dry gel particles were then added at concentrations of 10 g / hl, 20 g / hl, and 30 g / hl, and turbidity levels and reductions in sensitive proteins were measured as described in the Methods section above.

[0108] The results are shown in Table 4.

[0109]

[0110] Table 4

[0111] As can be seen from the above experiments, even at a dosage of only 10 g, the silica particles of the present invention can achieve most of the turbidity reduction achievable at loadings of 20 g / hl or 30 g / hl, demonstrating excellent efficiency and indicating that even lower levels can be used in practice. Furthermore, the reduced silica content is expected to lead to downstream processing benefits, as less refining material must be removed from beverage products.

[0112] Silica bodies with different particle sizes and pore volumes (Examples 31 and 32)

[0113] Two experiments were conducted to analyze the effects of different particle sizes or the use of silica particles with very high pore volumes on turbidity and reduction of sensitive proteins. As described above, wort samples were obtained during transfer from the wort tank to vortex settling. The wort consisted of 60% malt and 40% adjuvants (wort 3 as described above). Silica particles were then added at a concentration of 20 g / hl, and turbidity levels and reduction of sensitive proteins were measured as described in the Methods section above. The results are shown in Table 5.

[0114]

[0115] Table 5

[0116] As can be seen from the above experiments, all silica samples of the present invention showed a significant reduction in turbidity; however, dry gel 12 (Example 29) was superior to dry gels 16 and 17 (Examples 31 and 32, respectively) in terms of turbidity and protein reduction.

[0117] Industrial-scale implementation example (Example 33)

[0118] As described in the Methods section above, the use of porous silica particles in the production of beer with 60% malt and 40% adjuncts was tested.

[0119] Table 6 shows the measurements taken on the filter unit when filtering fermented beer obtained from a reference brew (40% adjunct beer) and an equivalent brew using silica desiccant particles. The reference brew and the brew using silica particles were separated into two tanks (C15-1 / C15-2 and Example 33-1 / 33-2, respectively), and the pressure differential in the filter was automatically measured using the filtration equipment. The properties of the silica desiccant particles used were the same as those provided in Example 21 (desiccant 12) described above.

[0120]

[0121] Table 6

[0122] The data show that brews using silica particles according to the invention have a lower load on the filter (based on ΔP value per 100 hl) than reference brews. In particular, Example 33-1 was able to filter twice the amount of beer with half the pressure change compared to Comparative Example C15-1.

[0123] Although the invention has been described in detail, it should be understood that various changes, substitutions, and modifications are contemplated without departing from the principles and scope of the invention. Therefore, appropriate equivalents should be considered to interpret the scope of the invention as defined herein, particularly the following claims. The terms “a,” “an,” and “the” do not exclude the presence of multiple indicators unless the context clearly specifies otherwise. Optional or alternatively means that a feature or activity may or may not be present. Either is contemplated. In embodiments, one or more optional features may be present. Alternatively, one or more optional features may not be present. A range herein may be expressed as “from” a particular value and / or “to” another particular value, and is intended to include the endpoints of the range.

Claims

1. Use of porous silica particles or porous precipitated silica particles in the treatment of wort, wherein the porous silica particles have a water content of 30% by weight or less and a pore volume of 0.4 ml / g or greater.

2. The use according to claim 1, wherein the porous silica particles have a pore volume of 0.75 ml / g or greater.

3. The use according to claim 2, wherein the porous silica particles have a pore volume of 1 ml / g or greater, optionally wherein the porous silica particles have a pore volume of 1.5 ml / g or greater.

4. The use according to any one of the preceding claims, wherein the porous silica particles have a pore volume of 2 ml / g or less, optionally wherein the porous silica particles have a pore volume of 1.8 ml / g or less.

5. The use according to any one of the preceding claims, wherein the porous silica particles have a water content of 20% by weight or less.

6. The use according to any one of the preceding claims, wherein the porous silica particles have a water content of 10% by weight or less, preferably 5% by weight or less.

7. The use according to any one of the preceding claims, wherein the porous silica particles are porous silica gel particles.

8. The use according to claim 7, wherein the porous silica gel particles are porous silica dry gel particles.

9. The use according to any one of the preceding claims, wherein the porous silica particles have a density of 800 μm. 2 / g or smaller surface area.

10. The use according to claim 9, wherein the porous silica particles have a density of 500 μm. 2 / g or smaller surface area.

11. The use according to any one of the preceding claims, wherein the porous silica particles are used in an amount of 1 g to 50 g per 100 liters of wort, optionally 10 g to 30 g per 100 liters of wort.

12. The use according to claim 11, wherein the porous silica particles are used in an amount not exceeding 25 g per 100 liters of wort, for example 20 g per 100 liters of wort.

13. The use according to any one of the preceding claims, wherein the porous silica particles have a median weight particle size (D50) of 1 μm or greater, optionally 5 μm or greater.

14. The use according to any one of the preceding claims, wherein the porous silica particles have a median weight particle size (D50) of 200 μm or less, 150 μm or less, 100 μm or less, 80 μm or less, or optionally 50 μm or less.

15. Methods for processing wort include: Contact the wort with porous silica particles or porous precipitated silica particles. The porous silica particles described herein have a water content of 30% by weight or less and a pore volume of 0.4 ml / g or greater.

16. The method of claim 15, wherein contact between the porous silica particles and the wort occurs in a mashing tank, a filter tank, a filter press, a wort pot, a vortex / decanter, or a fermenter, or between any two of the above.

17. The method of claim 15 or 16, further comprising causing the silica particles to settle out of the wort and separating the wort from the silica particles.

18. The method according to any one of claims 15 to 17, further comprising using the wort to produce a beverage.

19. Methods for preparing beverages, including: Processing grains to produce wort; Contact the wort with porous silica particles or porous precipitated silica particles. and The resulting wort is used to produce beverages. The porous silica particles described herein have a water content of 30% by weight or less and a pore volume of 0.4 ml / g or greater.

20. The method of claim 19, further comprising separating silica particles from the wort before using the wort to produce the beverage.

21. The method of claim 20, wherein the porous silica particles are separated from the wort together with waste grains produced from processed grains.

22. The method according to any one of claims 19 to 21, wherein the method for preparing the beverage is a method for brewing a fermented beverage, and comprises: Processing grains to produce wort; Contact the wort with porous silica particles or porous precipitated silica particles. and Fermented wort is used to produce fermented beverages.

23. The method of claim 22, wherein the fermented beverage is beer.

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