Preparation method of silicon dioxide for beer adsorbent

Abstract

The invention discloses a preparation method of silicon dioxide for a beer adsorbent, which belongs to a silicon dioxide preparation technology and comprises the following steps: S1, selecting solid water glass with modulus of 3.2-3.5, putting the solid water glass into a static pressure kettle, and preparing the solid water glass into a water glass solution with silicon dioxide content of 10wt%-15wt%; secondly, a sulfuric acid solution with the concentration being 10 wt%-20 wt% is prepared; the preparation method comprises the following steps: adding industrial purified water accounting for 1 / 5 of the volume of a reaction kettle into the reaction kettle, introducing steam, heating to 50 DEG C, then adding sodium bicarbonate accounting for 0.25-0.3 wt% of the industrial purified water and a prepared water glass solution, carrying out a first reaction, and finally adding a surfactant oligomeric sorbitol ester; by adding the surfactant oligomeric sorbitol ester, excessive aggregation of silicon dioxide particles in the reaction process is prevented, the generated silicon dioxide has a high specific area, and the effect of increasing the number of pores is achieved by utilizing the reaction of sodium bicarbonate and sulfuric acid in the acidification stage to produce carbon dioxide gas.

Description

Technical Field

[0001] The invention belongs to the technical field of silicon dioxide preparation, and in particular relates to a method for preparing silicon dioxide for beer adsorbent. Background Art

[0002] Beer is a fermented wine made from malt and water as the main raw materials, hops (including hop products), and yeast fermentation. It contains carbon dioxide and can form foam. Beer is a low-alcohol wine, containing carbon dioxide, multiple amino acids, vitamins, low-molecular sugars, inorganic salts and various enzymes. It has the effects of sterilization, fatigue relief, and digestion. The alcohol content is very low, and drinking beer is not easy to get drunk and hurt the body. Drinking a small amount will be good for your health. Because it contains sensitive proteins and polyphenols and other substances, it is easy to form non-biological turbidity. Turbidity in beer will shorten the shelf life of the product and affect its appearance and taste.

[0003] Silica is a porous material. Its main characteristics are large surface area, many pores, large structural space, low surface tension, small viscosity-temperature coefficient, high compressibility, high gas permeability, etc. Silica has been widely used in the beer industry as a new environmentally friendly adsorbent. It can effectively remove turbid proteins in beer without affecting the quality of beer products. Compared with other filter aids, silica has the advantages of less addition and better effect. For this reason, we propose a method for preparing silica for beer adsorbent. Summary of the invention

[0004] The present invention provides a method for preparing silicon dioxide for beer adsorbent to solve the problems raised in the above background technology.

[0005] To achieve the above object, the present invention provides the following technical solution: a method for preparing silicon dioxide for beer adsorbent, comprising the following steps:

[0006] S1, select solid water glass with a modulus of 3.2-3.5 and put it into a static autoclave to prepare a water glass solution with a silicon dioxide content of 10wt%-15wt%; then prepare a sulfuric acid solution with a concentration of 10wt%-20wt%;

[0007] S2, adding industrial purified water accounting for 1 / 5 of the volume of the reactor into the reactor, and introducing steam to raise the temperature to 50° C., then adding sodium bicarbonate accounting for 0.25wt%-0.3wt% of the industrial purified water and the prepared water glass solution, carrying out the first reaction, and finally adding the surfactant oligomeric sorbitol ester;

[0008] S3. In the first reaction process in S2, sodium silicate solution and sulfuric acid solution are added for stirring, and the reaction solution is added until the reaction solution accounts for 70% of the volume of the reactor, and the reaction temperature is maintained and the pH value is controlled during the stirring process;

[0009] S4, continue to drop sulfuric acid solution until the pH value of the reaction system is in the range of 3.0-4.0, at which time sodium bicarbonate reacts with sulfuric acid to generate carbon dioxide gas, and the reaction temperature is controlled in the range of 40°C-60°C to keep the stirring speed unchanged, and continue aging for 60 minutes after the reaction is completed;

[0010] S5. The reaction slurry is injected into a membrane filter press and washed with industrial clean water until the conductivity of the washed filtrate is less than 200 μs / cm; the filter cake is sent to a pulper and a colloid mill to be prepared into a concentrated slurry, and the concentrated slurry is centrifugally atomized into tiny droplets by a high-speed rotating atomizing disk, and dried with hot air generated by a natural gas combustion furnace to prepare a powdered product, and the moisture content of the product is controlled at 6.0%;

[0011] S6. Grind the product obtained in S5 with a high-pressure airflow mill to prepare a finished product with a particle size D50 of 5.0 μm-10.0 μm, thereby preparing nano-silica for beer anti-turbidity agent with high adsorption efficiency

[0012] Furthermore, in S1, the specific configuration method of the water glass solution is to select solid water glass with a modulus of 3.2-3.5 and put it into an autoclave, add steam to pressurize it to 0.8MPa-1.0MPa and maintain the pressure for 2 hours to obtain concentrated water glass, and add water to the concentrated water glass to obtain a water glass solution with a silicon dioxide content of 10wt%-15wt%, store it in a storage tank for more than 10 days, and use it after filtering.

[0013] Furthermore, in S2, when performing the first reaction, the pH value of the reaction solution needs to be controlled within the range of 9.0-10.0.

[0014] Furthermore, in S3, the stirring speed is controlled within the range of 50 r / min-100 r / min, the reaction temperature is maintained within the range of 30° C.-50° C., and the pH value is controlled within the range of 10-11.

[0015] Furthermore, in S4, sodium bicarbonate reacts with sulfuric acid to generate carbon dioxide gas which escapes, and the escaped carbon dioxide gas increases the number of pores in the silicon dioxide.

[0016] The beneficial effects of the present invention are:

[0017] By adding the surfactant oligosorbate, the excessive aggregation of silica particles is prevented during the reaction, so that the generated silica has a high specific area. In the acidification stage, sodium bicarbonate and sulfuric acid are reacted to produce carbon dioxide gas, thereby increasing the number of pores. DETAILED DESCRIPTION

[0018] In order to further understand the content, features and effects of the utility model of the present invention, the following embodiments are cited and described in detail as follows.

[0019] Embodiment 1:

[0020] A method for preparing silicon dioxide for beer adsorbent comprises the following steps:

[0021] S1. Select solid water glass with a modulus of 3.2-3.5 and put it into an autoclave, add steam to pressurize it to 0.8 MPa and maintain the pressure for 2 hours to obtain concentrated water glass, and add water to the concentrated water glass to obtain a water glass solution with a silicon dioxide content of 10wt%, and store it in a storage tank for more than 10 days, and use it after filtering; prepare a sulfuric acid solution with a concentration of 10wt%;

[0022] S2, adding industrial purified water accounting for 1 / 5 of the volume of the reactor into the reactor, and introducing steam to raise the temperature to 50°C, then adding sodium bicarbonate accounting for 0.25wt% of the industrial purified water and the prepared water glass solution, and performing the first reaction, and the pH value of the reaction solution needs to be controlled within the range of 9.0-10.0, and then finally adding the surfactant oligosorbate;

[0023] S3. In the first reaction process in S2, sodium silicate solution and sulfuric acid solution are added for stirring, and the reaction liquid is added until it accounts for 70% of the volume of the reactor, and when stirring, the stirring speed is controlled at 50r / min, the reaction temperature is maintained within the range of 30°C, and the pH value is controlled within the range of 10-11;

[0024] S4, continue to drop sulfuric acid solution until the pH value of the reaction system is in the range of 3.0-4.0, at which time sodium bicarbonate reacts with sulfuric acid to generate carbon dioxide gas that escapes, and the escaped carbon dioxide gas increases the number of pores in the silicon dioxide, and the reaction temperature is controlled within the range of 40°C to keep the stirring speed unchanged, and after the reaction is completed, continue aging for 60 minutes;

[0025] S5. The reaction slurry is injected into a membrane filter press and washed with industrial clean water until the conductivity of the washed filtrate is less than 200 μs / cm; the filter cake is sent to a pulper and a colloid mill to be prepared into a concentrated slurry, and the concentrated slurry is centrifugally atomized into tiny droplets by a high-speed rotating atomizing disk, and dried with hot air generated by a natural gas combustion furnace to prepare a powdered product, and the moisture content of the product is controlled at 6.0%;

[0026] S6. Grind the product obtained in S5 with a high-pressure airflow mill to prepare a finished product with a particle size D50 of 5.0 μm, thereby preparing nano-silica for beer anti-turbidity agent with high adsorption efficiency.

[0027] Embodiment 2:

[0028] S1. Select solid water glass with a modulus of 3.2-3.5 and put it into an autoclave, add steam to pressurize it to 0.9 MPa and maintain the pressure for 2 hours to obtain concentrated water glass, and add water to the concentrated water glass to obtain a water glass solution with a silicon dioxide content of 12wt%, and store it in a storage tank for more than 10 days, and use it after filtering; prepare a sulfuric acid solution with a concentration of 15wt%;

[0029] S2, adding industrial purified water accounting for 1 / 5 of the volume of the reactor into the reactor, and introducing steam to raise the temperature to 50°C, then adding sodium bicarbonate accounting for 0.27wt% of the industrial purified water and the prepared water glass solution, and performing the first reaction, and the pH value of the reaction solution needs to be controlled within the range of 9.0-10.0, and then finally adding the surfactant oligosorbate;

[0030] S3. In the first reaction process in S2, sodium silicate solution and sulfuric acid solution are added for stirring, and the reaction liquid is added until it accounts for 70% of the volume of the reactor, and when stirring, the stirring speed is controlled at 80r / min, the reaction temperature is maintained within the range of 40°C, and the pH value is controlled within the range of 10-11;

[0031] S4, continue to drop sulfuric acid solution until the pH value of the reaction system is in the range of 3.0-4.0, at which time sodium bicarbonate reacts with sulfuric acid to generate carbon dioxide gas that escapes, and the escaped carbon dioxide gas increases the number of pores in the silicon dioxide, and the reaction temperature is controlled within the range of 50°C to keep the stirring speed unchanged, and after the reaction is completed, continue aging for 60 minutes;

[0032] S5. The reaction slurry is injected into a membrane filter press and washed with industrial clean water until the conductivity of the washed filtrate is less than 200 μs / cm; the filter cake is sent to a pulper and a colloid mill to be prepared into a concentrated slurry, and the concentrated slurry is centrifugally atomized into tiny droplets by a high-speed rotating atomizing disk, and dried with hot air generated by a natural gas combustion furnace to prepare a powdered product, and the moisture content of the product is controlled at 6.0%;

[0033] S6. Grind the product obtained in S5 with a high-pressure airflow mill to prepare a finished product with a particle size D50 of 7.0 μm, thereby preparing nano-silica for beer anti-turbidity agent with high adsorption efficiency.

[0034] Embodiment three:

[0035] S1. Select solid water glass with a modulus of 3.2-3.5 and put it into an autoclave. Add steam to pressurize it to 1 MPa and maintain the pressure for 2 hours to obtain concentrated water glass. Add water to the concentrated water glass to obtain a water glass solution with a silicon dioxide content of 15 wt%. Store it in a storage tank for more than 10 days and use it after filtering. Prepare a sulfuric acid solution with a concentration of 20 wt%.

[0036] S2, adding industrial purified water accounting for 1 / 5 of the volume of the reactor into the reactor, and introducing steam to raise the temperature to 50° C., then adding sodium bicarbonate accounting for 0.3wt% of the industrial purified water and the prepared water glass solution, and performing the first reaction, and the pH value of the reaction solution needs to be controlled within the range of 9.0-10.0, and then finally adding the surfactant oligosorbate;

[0037] S3. In the first reaction process in S2, sodium silicate solution and sulfuric acid solution are added for stirring, and the reaction liquid is added until it accounts for 70% of the volume of the reactor, and when stirring, the stirring speed is controlled at 100 r / min, the reaction temperature is maintained within the range of 50° C., and the pH value is controlled within the range of 10-11;

[0038] S4, continue to drop sulfuric acid solution until the pH value of the reaction system is in the range of 3.0-4.0, at which time sodium bicarbonate reacts with sulfuric acid to generate carbon dioxide gas that escapes, and the escaped carbon dioxide gas increases the number of pores in the silicon dioxide, and the reaction temperature is controlled within the range of 60°C to keep the stirring speed unchanged, and after the reaction is completed, continue aging for 60 minutes;

[0039] S5. The reaction slurry is injected into a membrane filter press and washed with industrial clean water until the conductivity of the washed filtrate is less than 200 μs / cm; the filter cake is sent to a pulper and a colloid mill to be prepared into a concentrated slurry, and the concentrated slurry is centrifugally atomized into tiny droplets by a high-speed rotating atomizing disk, and dried with hot air generated by a natural gas combustion furnace to prepare a powdered product, and the moisture content of the product is controlled at 6.0%;

[0040] S6. Grind the product obtained in S5 with a high-pressure airflow mill to prepare a finished product with a particle size D50 of 10.0 μm, thereby preparing nano-silica for beer anti-turbidity agent with high adsorption efficiency.

[0041] Table 1 Silicon dioxide of Examples 1 to 3

[0042]

[0043]

[0044] It can be seen from the above embodiments that the method of the present invention can achieve the preparation of silica with BET in the range of 600-700m2 / g; median diameter (D50) 5um-10um; silica content ≥95-98%; and CTAB: 500-600m2 / g.

[0045] The above shows and describes the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited by the above embodiments. The above embodiments and descriptions are only preferred examples of the present invention and are not intended to limit the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, which fall within the scope of the present invention. The scope of protection of the present invention is defined by the attached claims and their equivalents.

Claims

1. A method for preparing silicon dioxide for beer adsorbent, Features: The following steps are involved: S1, select solid water glass with a modulus of 3.2-3.5 and put it into a static autoclave to prepare a water glass solution with a silicon dioxide content of 10wt%-15wt%; then prepare a sulfuric acid solution with a concentration of 10wt%-20wt%; S2, adding industrial purified water accounting for 1 / 5 of the volume of the reactor into the reactor, and introducing steam to raise the temperature to 50° C., then adding sodium bicarbonate accounting for 0.25wt%-0.3wt% of the industrial purified water and the prepared water glass solution, carrying out the first reaction, and finally adding the surfactant oligomeric sorbitol ester; S3. In the first reaction process in S2, sodium silicate solution and sulfuric acid solution are added for stirring, and the reaction solution is added until the reaction solution accounts for 70% of the volume of the reactor, and the reaction temperature is maintained and the pH value is controlled during the stirring process; S4, continue to drop sulfuric acid solution until the pH value of the reaction system is in the range of 3.0-4.0, at which time sodium bicarbonate reacts with sulfuric acid to generate carbon dioxide gas, and the reaction temperature is controlled in the range of 40°C-60°C to keep the stirring speed unchanged, and continue aging for 60 minutes after the reaction is completed; S5. The reaction slurry is injected into a membrane filter press and washed with industrial clean water until the conductivity of the washed filtrate is less than 200 μs / cm; the filter cake is sent to a pulper and a colloid mill to be prepared into a concentrated slurry, and the concentrated slurry is centrifugally atomized into tiny droplets by a high-speed rotating atomizing disk, and dried with hot air generated by a natural gas combustion furnace to prepare a powdered product, and the moisture content of the product is controlled at 6.0%; S6. Grind the product obtained in S5 with a high-pressure airflow mill to prepare a finished product with a particle size D50 of 5.0 μm-10.0 μm, thereby preparing nano-silica for beer anti-turbidity agent with high adsorption efficiency.

2. A method for preparing silicon dioxide for beer adsorbent according to claim 1, Features: The specific configuration method of the water glass solution in S1 is to select solid water glass with a modulus of 3.2-3.5 and put it into an autoclave, add steam to pressurize it to 0.8MPa-1.0MPa and maintain the pressure for 2 hours to obtain concentrated water glass, and add water to the concentrated water glass to obtain a water glass solution with a silicon dioxide content of 10wt%-15wt%, store it in a storage tank for more than 10 days, and use it after filtering.

3. A method for preparing silicon dioxide for beer adsorbent according to claim 1, Features: In the step S2, when performing the first reaction, the pH value of the reaction solution needs to be controlled within the range of 9.0-10.

0.

4. A method for preparing silicon dioxide for beer adsorbent according to claim 1, Features: In S3, the stirring speed is controlled within the range of 50 r / min-100 r / min, the reaction temperature is maintained within the range of 30° C.-50° C., and the pH value is controlled within the range of 10-11.

5. A method for preparing silicon dioxide for beer adsorbent according to claim 1, Features: In the S4, sodium bicarbonate reacts with sulfuric acid to generate carbon dioxide gas which escapes, and the escaped carbon dioxide gas increases the number of pores in the silicon dioxide.

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