JPH0597421A - Production of silica gel for stabilization treatment of beer - Google Patents

Abstract

PURPOSE:To produce silica xerogel which adsorbs and removes protein causing turbidity to beer but hardly adsorbs foaming protein and to produce beer having satisfactory stability and foam retentivity. CONSTITUTION:Silica hydrogel obtd. by neutralizing an aq. alkali silicate soln. with an acid is converted into silica xerogel by drying and this xerogel is fired at 150-450 deg.C in a steam atmosphere to produce silica gel for stabilization treatment of beer.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing silica gel for beer stabilizing treatment, which is used for producing beer having good stability and foam-holding property.

[0002]

2. Description of the Related Art Beer is a container (bottle, can, barrel, etc.)
After being filled in, it may become cloudy when it is stored for a long period of time or when it is cooled. This turbidity is caused by the association of certain proteins in beer and colloidal components such as polyphenols. Beer that is stable and does not generate such turbidity is desired. Also,
Foam retention is also important as the commercial value of beer. The foam is formed by combining a protein (foaming protein) and a component such as a saccharide to form a film.

Conventionally, as means for improving the stability of beer, an enzyme method (papain method), a tannic acid method, PVP
The P method, the silica gel method and the like are used. In this,
The silica gel method is widely used because it is inexpensive and does not adversely affect the taste and aroma of beer. In the silica gel method, silica gel is generally added to beer at the final stage of beer production, components (mainly proteins) that cause turbidity are adsorbed on the silica gel, and then this silica gel is removed by a filter.

[0004] For example, British Patent No. 938153, British Patent No. 981715 and the like describe a method of using silica xerogel as silica gel, but the stabilizing effect of beer was not sufficient. Further, Japanese Patent Publication No. 63-38188 discloses a method of using a calcined silica xerogel. Even in this method, the effect of stabilizing beer is not always sufficient, the baking temperature is as high as 450 ° C. to 750 ° C., and the baking time is as long as 6 hours, which is a problem in terms of economy as an industrial manufacturing method. is there. Further, the conventional silica xerogel has a problem that the foamability of the obtained beer is generally insufficient.

On the other hand, when silica hydrogel is used,
Although beer had good foam retention, the stability of beer was insufficient. In addition, since silica hydrogel contains a large amount of water, there is a problem that mold or the like is likely to occur.

[0006]

DISCLOSURE OF THE INVENTION The present invention provides a method for producing silica gel in which proteins causing turbidity of beer are adsorbed and removed and adsorption of foaming proteins is extremely small, and the stability is good and The purpose is to produce beer with good foam retention.

[0007]

The present invention provides a method for producing silica gel for beer stabilization, which comprises drying silica hydrogel into a xerogel by drying and then calcining it in a steam atmosphere. is there.

The method for producing silica hydrogel is not particularly limited, and silica hydrogel produced by various methods can be used. For example, a method of neutralizing an aqueous alkali silicate solution with an acid can be preferably adopted. For example, an alkaline silicate aqueous solution such as sodium silicate or potassium silicate and an aqueous solution of a mineral acid such as sulfuric acid or hydrochloric acid are uniformly mixed at a certain ratio, speed, temperature, etc. to form a gel, and aging is carried out if necessary. , Silica hydrogels can be produced.

The silica hydrogel thus obtained is appropriately washed with water and dried to obtain a silica xerogel. After drying, or at the same time as the drying process,
It is preferable to pulverize the silica gel into fine particles.

When firing in a steam atmosphere, the silica gel needs to be a xerogel that has been subjected to a drying step in advance. However, when the hydrogel is introduced into the firing step as it is, the xerogel was first formed by drying. It will be fired later.

The silica gel produced by the method of the present invention is preferably in the form of fine particles having an average particle diameter of about 5 to 30 μm. As the pore characteristics of silica gel, the average particle diameter is 5 to 30 μm and the pore volume is 0.8 to 1.8.
ml / g, average pore diameter of 60 to 180Å, and specific surface area of 200 to 700 m ² / g are preferable in terms of beer stabilization treatment performance and filterability. The pore characteristics do not change significantly by firing in a steam atmosphere, but the pore characteristics are those after firing.

In the present invention, the water vapor concentration in the atmosphere during firing is 20 to 100% by volume, preferably 50 to 10%.
0% by volume is desirable. Under the condition that the concentration of water vapor is less than 20% by volume, the effect of water vapor in the atmosphere may not be sufficiently exhibited, which is not preferable. Various methods can be adopted as the method of controlling the atmosphere during firing to the above range. For example, steam generated from a boiler or the like is introduced alone or after mixing air at a predetermined ratio and then introduced into a firing furnace, or after passing air through water controlled to a certain temperature, a gas containing steam generated. Can be introduced into the firing furnace, or another method can be used.

The pressure during firing is close to the atmospheric pressure when a normal firing apparatus is used, but the effect of the present invention can be exhibited by introducing steam even under pressure or under reduced pressure. is there. In this case, the partial pressure of water vapor is preferably 0.2 atm or more.

In the present invention, the firing temperature is 150 ° C to 4 ° C.
It is preferably 50 ° C. If the firing temperature is lower than 150 ° C., the effect of water vapor in the atmosphere is not significant and the firing time may be long, which is not preferable. The firing temperature of 300 ° C. or higher is more preferable because the firing time can be shortened. If the firing temperature is higher than 450 ° C, the substantial effect is equivalent to 450 ° C or lower, and further effects cannot be obtained, and there is a possibility that a high heat resistance is required for the firing device, which is not preferable. ..

In the present invention, the apparatus used when firing the silica xerogel is not particularly limited as long as it can be controlled in a water vapor atmosphere. For example, a firing device such as a rotary kiln, a tunnel furnace, a muffle furnace, or the like can be used.

[0016]

[Action] Although the action of water vapor in the atmosphere during firing is not always clear, the reaction with the silica gel surface selectively adsorbs proteins that cause turbidity, and the proteins required for bubble formation are It is considered that this contributes to the generation of a surface state that is difficult to adsorb.

When the infrared absorption spectrum which is considered to be related to the surface state of silica gel is measured, there are several different types of silanol groups on the surface of silica xerogel. In particular, the rate of reduction of hydrogen-bonded silanol groups is
Compared with generally-calcined in air, it greatly increases by calcining in a steam atmosphere. Therefore, steam has a catalytic effect in the dehydration process (condensation process of surface silanol groups) of silica xerogel during calcining. Then, it is considered that the surface state is generated at a low firing temperature and a short firing time.

[0018]

Example: No. 3 sodium silicate having a SiO ₂ concentration of 5
A silica gel slurry was prepared by diluting the mixture with demineralized water so as to have a weight percentage and adding 20 wt% sulfuric acid. This slurry was washed with water and dehydrated using a centrifuge, and then at 110 ° C.
The powder was pulverized and dried with a gas stream dryer to obtain silica xerogel (this is referred to as silica gel 1).

This silica gel 1 was fired in a muffle furnace in the atmosphere shown in Table 1 at a temperature and for a time to obtain silica gels 2-9. Atmospheric pressure is atmospheric pressure, silica gel 4 ~
In 6, the atmospheric component other than water vapor is air. Here, silica gels 2 to 6 are the silica gel of the present invention.

[0020]

[Table 1]

Various physical properties of the above-mentioned silica gels 1 to 9, commercially available silica xerogel for beer stabilization treatment (commercial gel 1), and silica hydrogel for beer stabilization treatment (commercial gel 2) were measured by the following methods. The results are shown in Table 2.

(Average particle diameter) Using a Coulter counter (manufactured by Nikkaki Co .; Coulter Multisizer),
It was measured by a method of determining the particle size from the change in electric resistance value generated when the suspended particles in the electrolytic solution pass through the aperture (pore).

(Pore volume, average pore diameter, specific surface area) O
The pore volume was measured by the nitrogen adsorption method using an omnisorp 100 manufactured by MICRON, and the average pore diameter was determined by the 50% volume diameter. The specific surface area was determined by the nitrogen adsorption BET method.

(Water content) Each silica gel was obtained from the weight loss when dried at 180 ° C., and expressed as a wet weight standard weight%.

[0025]

[Table 2]

Next, silica gels 1 to 9 and commercially available gels 1 and 2
Was used to carry out a beer stabilization test. Commercial beer was used as beer for evaluation. The stabilization treatment was performed by adding 800 ppm of silica gel and 1200 ppm of diatomaceous earth (filter aid) to beer, contacting them for 5 minutes, and then filtering with a filter. The stability and foam retention of this stabilized beer were measured in the following manner and are shown in Table 3 in comparison with untreated beer.

(Stability) Stabilized beer and untreated beer (commercial beer) were stored in a constant temperature bath at 50 ° C. for 5 days, and subsequently cooled in a constant temperature bath at 0 ° C. for 1 day, and then turbid. The degree was measured in EBC units (cold turbidity). The lower the turbidity, the better the stability of the beer. As the turbidimeter, Sigmalist KTL30-21 manufactured by Tokyo Sangyo Co., Ltd. was used.

(Bubble-holding property) As to beer after stabilization treatment and untreated beer, the Sigma method (METHOD OF OF
ANALYSIS OF THE AMERICAN SOCIETY OF BREWING CHEMI
The sigma value was measured according to STS BEER-22). The higher the sigma value, the better the foam retention of beer.

[0029]

[Table 3]

[0030]

Industrial Applicability According to the method of the present invention, silica gel for beer stabilization treatment used for producing beer having good durability and foam-holding property can be produced at a low firing temperature and a short firing time. The silica gel produced by this method selectively adsorbs and removes proteins that cause turbidity, and has very little adsorption of foamed proteins.

Claims (7)

[Claims] 1. A method for producing silica gel for beer stabilizing treatment, which comprises drying silica hydrogel into a xerogel and then calcining it in a steam atmosphere. 2. The method for producing silica gel for beer stabilization according to claim 1, wherein the silica hydrogel is obtained by neutralizing an aqueous alkali silicate solution with an acid. 3. Water vapor of 20 to 100 in the atmosphere during firing.
The method for producing silica gel for beer stabilizing treatment according to claim 1 or 2, wherein the silica gel is contained in a volume percentage. 4. The partial pressure of water vapor in the atmosphere during firing is 0.2.
The method for producing silica gel for beer stabilization according to any one of claims 1 to 3, wherein the pressure is not less than atmospheric pressure. 5. The method for producing silica gel for beer stabilization according to claim 1, wherein the baking temperature is 150 to 450 ° C. 6. The silica gel after the calcination treatment has an average particle diameter of 5 to 30 μm, a pore volume of 0.8 to 1.8 ml / g, an average pore diameter of 60 to 180Å, and a specific surface area of 200 to 700 m ^2.
/ G, The method for producing silica gel for beer stabilization according to any one of claims 1 to 5. 7. A method for stabilizing beer by contacting the silica gel obtained by the production method according to claim 1 with beer and then separating the beer.