DE1954230A1 - Method of treating beer - Google Patents

Description

The present invention relates to a method of treatment of beer and, in particular, a method of improving beer by reducing its tendency to Fogging during storage.

The term "beer" in this description is to be understood in a broad sense and includes beverages in the English style Ale, lagers, strong beers (stout beers) and other liquids with which there are fogging problems in storage there.

Various methods of clarifying beer by removing the various fogging components have heretofore been proposed. The haze or cloudiness present in beer can sometimes be removed by filtration methods, but in some beers haze or cloudiness develops again when standing, and if the beer has already been filled into bottles or cans, these imperfections are generally not feasible. it is therefore desirable, both during manufacture or while standing before the last Verarbeitungestufe developed Sohleier and schleiderbildende substances which su Schleierbil-

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during the storage of the beer after the last processing step, but before consumption, to remove. It is desirable for the treatment of the beer used materials from the beer none Remove components that are essential for the character of the beer, e.g. slug-forming components, coloring Components and foam crown-forming components.

Various ^ substances such as B. Bentonite, activated carbon, nylon, · .. Polyvinyl pyrrolidone and certain silicas (silica anhydrides) have heretofore been proposed for this purpose and are effective to a greater or lesser extent. However, the cost of such treatment is both from the fabrics themselves as well as from the processing, such as ζ. Β., Filtration and storage, arise from, not insignificant and any cost reduction is tempting, especially when it is accompanied by increased effectiveness a loss of desired properties, such as taste and foam head retention, is not required * moreover demand some legal regulations about food purity that drinks are not added to soluble substances.

It has now been found that certain silica xerogels with large surface and a rather narrowly defined cement pore diameter (MPD) good results regarding Fog removal and no adverse effect on the preservation of the head of foam, even in some Cases improve this special property of the beer.

Accordingly, the present invention provides a method for treating beer with a silica gel under the following Separation of the silica from the beer and the process is characterized in that it is the Silica gel around a xerogel with a surface in between

P 2

700 m / g and 1200 m / g and a mean pore diameter

from 25 - 150 S.

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An accepted test method for the haze-reducing or stabilizing effect of silicas used in the treatment of beers is a precipitation test with saturated aramonium sulphate solution, the so-called SASPL test (Saturated Ammonium Sulphnte Precipitation Limit) In this test, saturated ammonium sulphate solution samples of treated and untreated samples Beer is added and the amount of solution required to cause a sudden increase in turbidity, measured by a reflectometer, is determined a hatred of the fog-reducing effectiveness of the silica to be tested

The foam head retention values, HRV (Head Retention Values), referred to in this description have been determined in the following way:

Samples of beer were made at 0 ° C with a sample of silica (1 β as GiOg d © liters) treated and 5 minutes or left for 24 hours. Then became the silica filtered off. The treated beer was carefully allowed to run into a pipe up to a height of 10 cm Tube possessed a? At its lower end? sintered glass pane, through which carbon dioxide g '· s for the purpose of forming a The head of foam in the beer could become pearly pearls. That The bubbling in of the gas is continued up to a predetermined height (32.5 era) and then the gas supply is reduced to a hatred, in order to like the beer on the disk to stop, whereupon the 3chnum begins to fall The IIRV is that multiplied by 1.44 and expressed in seconds Time that passes for the boundary between the level of the liquid beer and the 3odenflache of the Foam between the markings at 5 and 7 »5 cm passes on the pipe.

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Although the following theory is by no means binding wants, it seems to give a possible explanation for the functioning of the method according to the invention. It appears namely possible that the stability of foam on beer by a positive or reinforcing and a negative or suppressive Schnumkronefnktor dependent and these two factors are represented by substances which have significantly different particle size or shape, so you might get through Choosing an Eieselde xerogel with a narrowly defined one LIPD can preferentially or selectively remove the negative factor.

In a preferred embodiment of the present invention the LIPD of the silica xerogel has a 7 / ert of 40 - 80 Ä.

It will be understood that the UFD is an average and can be the result of a broad or a narrow actual distribution of pore sizes. The silicas preferred for use in the present invention have a broad distribution of pore sizes rather than a relatively narrow one, as is the case with the high volume xerogels proposed heretofore and with certain precipitated silicic acid nhydrides which have been assigned "mean pore diameters ¹¹ ".

For the purpose of the method according to the invention to work effectively and especially for the purpose of obtaining optimal results in terms of contact time between beer and silica and in terms of ease of separation of the beer of the silica, it is desirable that a significant proportion of the silica be present as fine particles. The average particle size of the silica is preferably less than 20 liqueurs.

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As in the case of the HPD above, the actual particles on which the average value is based can be in different '.' / be formed and for the inventive In the process, it is desirable that at least 10% by weight of the silica consist of particles that are smaller than 10 microns. True measurement of particle size is difficult if the particles are smaller than approximately 5 microns, on the other hand it has been found that in the interests of good Y values for Δml SASPL it is desirable that a significant number of particles are smaller than 5 microns

Accordingly, silica xerogels are at least 10 wt. # Of particles smaller than 5 microns, especially good usable.

The amount of silica used in treating beer is to some extent different from that actually chosen Xerogel and depending on the quality and age of the beer to be treated · In general, it becomes when used of the silica xerogel defined above normally it is not necessary to use more than 1 g of silica per liter of beer to be treated.

Suitable for use in the present invention Xerogels can be made by a variety of methods. A preferred process is a continuous one Process in which silica is formed by mixing an acid with sodium silicate under high shear conditions will be produced. With this procedure, one leaves an alkali silicone and an acid solution under high shear force react with each other · The silica produced can easily be washed acidic in a hydrogel larger surface and larger pore volume than that to give original silica and this Bydrogel delivers a xerogel when drying and crushing, wel-

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ches the properties that it possesses for dns according to the invention Making the process usable

Samples 1-5 in Table I below were used prepared by the preferred method, the acid and the silicate reacted with each other under high shear

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Table I.

rehearse 1 2 3 4th 4a 4b 5 Sodium silicate (HapOiSiOj, 1: 3 * 3)
SiOi content> j 25.2 25.2 25.2 25.2 25.2 25.2 sulfuric acid normality 10.8 10.8 11.4 11.4 11.4 11.4 pH on gelation 1.5 3.0 8.5 6.5 6.5 8.5 Hydrogel weight
kg 90.8 90.8 90.8 90.8 90.8 100 g Wn RfthmA fchnd et Hydrogel Hydrogel As for 2, how how Hydrogel with 30 minutes 30 minutes but under for 3 for 3 400 g 0.2 η long at 60Ό long in 227 1 . use sulfuric acid in 454 1 fee sulfuric acid of 0.1 η at 25 ° 25 Wed ser aged, at 20O C ge sulfur ■ grooves long ge 1. Sulfur-free wash with acid wash, then 'sdt IsLtucgswas- Pipe what with deioni- scr quick so, ser enilfat- conditioned water ? ^ pwr, aclH3 stft free Gewa for sulfatent 45-M lean ting distance gewa (W / v) ting 3 »sulfBtfreL sit Drying like 1 like 1 like 1 like 1 Tranael tlahlen itl J 1, iitH 0 9 throb oifeiit & trodcnet
λαλΟ f% mill <Mr4 A ⁴ I. cUU v / 175 "* 200 U mtthela InftsirahV Hammer- mill like fy- Liühle drogÄ3 before Pffaruaauimma '

Samples 6-8 were in lots application into a cup -having to "a pit llischers high shear made · The details are listed in fabeile II.

Table H J

rehearse 6th 9.3 7th 8th Sulfuric acid formality 40 9.3 3.6 VoI (cc) 21.4 50 50 Sodium silicate % SiO ₂ 21.4 9.9 VoI (cc) 160 Silicate solution. 8.0 200 200 Gelation pH 100 7.8 8.5 Hydrofcel weight κ 45 100 100 Aging time (Hin.) 120 120 Sulfuric Acid Treatment R. 0.2 normality 400 0.2 0.2 VoI (cc) 20th 400 400 Tearp. (° O) 30th 20th 20th Contact time (Jlin ·) 30th 30th

The sodium silicate was added to the sulfuric acid and it was vigorously stirred with a mixer, type Silverson. After the hydrogel was treated with acid, The bulk of the sulfate was removed by pouching with deionized Water (skin temperature) removed, followed by Oven drying at 200 ° C.

Samples of the various silicas from Tables I and II turned light-colored for their stabilizing effect Ale, as it is usually sold as bottled beer, evaluated, 1 g SiOg i) e liter of beer was used and the results are shown in Table III.

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Di · Kieselde can the beer in more convenient Velse el · a Aqueous suspension is set and then after, for example, 5 minutes EoataktMlt by filtration, if desired in the presence of a filter aid, separated are · Sin · different way of working 1st s «B«, stir the silica into the beer and then drink the beer, after the silica has settled

Tabel

Silica
sample surface Pore
■ vDluaen
cö / g UPD % I.
By
schnittli
ch © part
small size
μ Δ ml 1 837 0.89 43 13.7 1.9 2 930 0.70 31 2-5 2.2 3 715 1.10 62 2.4 2.4 4th 795 1.01 51 14th 2.1 4a 769 0.97 50 2.2 2.5 4b 775 0.94 49 12.2 1.8 VJl 794 1.17 59 17.9 2.1 6th 943 0.89 38 25.9 1.7 7th 819 0.93 45 24.7 1 # 7 8th 890 0.71 32 24.2 1.8

Further slopes of samples 4 and 4a were made for mold semi-technical «ilassetab applied in a brewery · Bs 2 g / 1 were used, the beer was "· look around." a light ale The results are shown in Table IV.

net

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Table 17

Control Sample 4 Sample 4a SASPLmI 0.9 3.0 3.2 Δ & 1 SASFL 0 2.1 2.3 HHV 132 127 127 Bitter value 19.0 20.2 18.8 Total Ng ppm 371 330 340 Lundin A Group, Durchsehnftfc 100 53 62

The results in Table IV indicate that the use of xerogels in accordance with the present invention had no significant effect on the taste expressed as the bitter value. The bitter value is determined as der- laohuaulongehnlt *

The decrease in the lundine fraction is a further indication of the useful haze-removing properties of these silicas. Lundin (J. Int. Brewing 1931st Vol 37) has developed a method of nitrogen fractionation _f which separates proteins according to their Uolekulargewioht. Me Lundin-Praktion A is the protein precipitated by tannin and provides the high-molecular nitrogen compounds . which · are responsible for the formation of egg eggs. A decrease in this fraction indicates a decrease in the fog-forming protein.

Passes practically no change in HSV shows indicate that there are no problems in this regard.

Brewery tests were carried out with further samples of silica xerogel. The beer used was eia light ale made in a semi-technical facility the brewery. Comparative experiments have been

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including fOhrt _f a Eontrolle without silica addition, an attempt old commercially available xerogel (Xerogel C) and tests nit different xerogels of the present invention · There per liter of 2 g of xerogel, calculated SiO ₂ used as a * · The results are shown in Table 7 ·

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Table V

ι control surface
m ² / g Pores
volume
cc / g MPD
1 By
cut
liche
Particle
size Jl total SASPL-Te st HRV
Sec. «, ■ _ _ 464 SASPL ml / 10 ml 128 Serogel C 470 0.6
AmI 127 360 0.92 103 23.4 426 1 * 3 127 Sample 1 426 127 83? 0.89 43 13 * 7 436 1 * 3 128 Sample 3 436 125 715 1.10 62 2.4 432 1.8 119 Sample 4b 424 122 775 0.94 49 12.2 426 1.25 122 448 123

N> CO O

Claims (1)

Claims 1, a method for treating beer with a silica gel with subsequent separation of the silica from the beer, characterized in that "the silica gel is a xerogel with a surface area between 700 m / s and 1200 m / g and an average pore diameter of 25 - 150 % acts. » 2, Verfnhran according to claim 1, characterized in that the mean pore diameter of silica 40 - 80 λ amounts to. 3 »Method according to claim 1 or 2, characterized in that that is, the average particle size of the silica tveniger nls is 20 microns. Method according to claims 3 to _9, characterized in that at least 10% by weight of the xerogel consist of particles smaller than 10 l'icrons. 5, method according to claim 4, characterized in that .at least 10 wt. # of the xerogel from particles smaller pass as 5 uikron 6 * method according to one of the preceding claims, characterized in that the distribution of the pore sizes, on which the mean pore diameter is based, is a broad. 009828/0969