CN104030298B - A kind of preparation method of beer silica gel - Google Patents
A kind of preparation method of beer silica gel Download PDFInfo
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- CN104030298B CN104030298B CN201410231341.XA CN201410231341A CN104030298B CN 104030298 B CN104030298 B CN 104030298B CN 201410231341 A CN201410231341 A CN 201410231341A CN 104030298 B CN104030298 B CN 104030298B
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Abstract
A preparation method for beer silica gel, its step comprises: 1) mixed with water by glycerine, and the mass ratio of glycerine and water is 1:(20-200); 2) step 1 is got) glycerine of gained and the mixed solution V1L of water, under the condition stirred, add sodium silicate solution, the volumetric molar concentration of described sodium silicate solution is 1.0-1.2mol/L, the pH of mixed solution is transferred to 8-10, adds water glass and sulphuric acid soln, keep the pH of mixed solution at 8-10, when sodium silicate solution adds V2L altogether, wherein V1=V2; 3) continuation interpolation sulphuric acid soln is 2-3 to the pH of mixed solution; 4) stir, then ageing; 5) wash, dry, then pulverize and obtain beer silica gel.Preparation method of the present invention, production technique is simple, and step is few, adds auxiliary agent few, is applicable to Workshop Production, and the pore volume of the silica gel obtained by preparation method of the present invention is large, and specific surface area is large, and pore size distribution is narrow, and absorption property is strong.
Description
Technical field
The present invention relates to silica gel field, particularly a kind of preparation method of beer silica gel.
Background technology
Beer silica gel is the filtering product of a class for beer filtration, is the pressed powder of a kind of non-crystalline state, multi-cellular structure.Because silica gel is easy to the protein of the muddiness of adsorbing in removing beer and muddy polyphenol polymer, plays the effect that peculiar smell is removed in the removal of impurity, can improve the quality of beer, the advantages such as the quality guaranteed period of prolongation beer and storage period, are widely used in the manufacture of beer.
Current generation gel-immersion operation (improvement operation)-aging process-washing step-baking operation, complex process, and the adsorptivity heterogeneity of product, the shortcomings such as pore size distribution is wide, and specific surface area is little.
Summary of the invention
In sum, the present invention is necessary the preparation method providing a kind of beer silica gel, and described preparation method's technique is simple, and the silica gel adsorption prepared is homogeneous, and pore size distribution is narrow, and specific surface area is large, and pore volume is large.
A preparation method for beer silica gel, its step comprises:
1) mixed with water by glycerine, the mass ratio of glycerine and water is 1:(20-200);
2) step 1 is got) glycerine of gained and the mixed solution V of water
1l, under the condition stirred, add sodium silicate solution, the volumetric molar concentration of described sodium silicate solution is 1.0-1.2mol/L, and the pH of mixed solution is transferred to 8-10, adds water glass and sulphuric acid soln, keeps the pH of mixed solution at 8-10, when sodium silicate solution adds V altogether
2l, wherein V
1=V
2;
3) continuation interpolation sulphuric acid soln is 2-3 to the pH of mixed solution;
4) stir, then ageing;
5) wash, dry, then pulverize and obtain beer silica gel.
Altogether, described step 1) be specially: water is heated to 60-80 DEG C, then is added to the water by glycerine, constant temperature stirs 5-10 minute.
Wherein, described step 2) described in the volumetric molar concentration of sulphuric acid soln be 4-4.2mol/L.
Preferably, described step 2) volumetric molar concentration of described sodium silicate solution is 1-1.2mol/L, the volumetric molar concentration of described sulphuric acid soln is 4-4.2mol/L.
Wherein, described step 2) agitation condition specifically: the rotating speed of stirring rake is 200-500r/min.
Wherein, described step 4) be specially, stir 1.5 hours under the constant temperature of 60-90 DEG C, the rotating speed 200-250rr/min of stirring rake.
Wherein, described step 2) the interpolation speed received of mesosilicic acid is 6000-11000L/h.
Compare prior art, preparation method of the present invention, production technique is simple, and step is few, adds auxiliary agent few, is applicable to Workshop Production, and the pore volume of the silica gel obtained by preparation method of the present invention is large, and specific surface area is large, and pore size distribution is narrow, and absorption property is strong.
Embodiment
Below in conjunction with some embodiments, the preparation method to beer silica gel of the present invention is described further.Specific embodiment is for further describing the present invention, non-limiting protection scope of the present invention.
The present invention's feature used is all from commercially available.
Detection method used by following examples has:
Opening size test: the absorption aperture normal distribution of test sample, testing method is multiple spot BET method, adopts the method for standard GB.T19587-2004 to detect, and the particle of statistics particle diameter within the scope of 10-15nm accounts for the per-cent of sample total amount;
Pore volume is tested: the single-point absorption total pore volume of test sample, and testing method is multiple spot BET method, adopts the method for standard GB.T19587-2004 to detect;
Specific surface area: BET multiple spot specific surface area, testing method is multiple spot BET method, adopts the method for standard GB.T19587-2004 to detect;
Absorption property is tested: micro-Kjeldahl, and concrete grammar gets the silica gel that 1000ml beer adds 300ppm, leave standstill two beer samples before and after detecting after 2 hours or dissolubility nitrogen content, and content is lower, shows that the ability of Silica eluent protein is stronger.
Embodiment 1
10m is added in container
3water as end liquid, be placed in water-bath and be heated to 60 DEG C, then in reactor, add glycerine 50kg, constant temperature stir 5min;
Get the mixed solution of the above-mentioned water of 1000L and glycerine, stirring velocity is set as 200r/min, dripping volumetric molar concentration toward reactor is the sodium silicate solution of 1mol/L, the pH value of reaction solution is adjusted to 8, and then to add volumetric molar concentration be the sodium silicate solution of 1mol/L and volumetric molar concentration is simultaneously the sulphuric acid soln of 4mol/L, and continues to drip sodium silicate solution, control process pH value is 8 ~ 10, the total addition level of sodium silicate solution is 1000L, adds complete, and the interpolation speed of sodium silicate solution is 6000L/h;
Continuation dropping sulfuric acid to terminal pH value is 2.5;
After completion of the reaction, the speed of stirring rake is reduced to 250r/min, 60 DEG C of constant temperature, ageing 1.5 hours;
Washing, dry, pulverizing.
Obtained beer silica gel is carried out opening size test, pore volume test, specific surface area and absorption property test, test result is listed in the table below.
Embodiment 2
10m is added in container
3water as end liquid, be placed in water-bath and be heated to 60 DEG C, then in reactor, add appropriate glycerine 500kg, constant temperature stir 10min;
Get the mixed solution of the above-mentioned water of 1000L and glycerine, on stirring velocity is set as 250r/min, dripping volumetric molar concentration toward reactor is the sodium silicate solution of 1.2mol/L, the pH value of reaction solution is adjusted to 10, then to add volumetric molar concentration be the sodium silicate solution of 1.2mol/L and volumetric molar concentration is simultaneously the sulphuric acid soln of 4mol/L, and continue to drip sodium silicate solution, control process pH value is 8 ~ 10, the total addition level of sodium silicate solution is 1000L, add complete, the interpolation speed of sodium silicate solution is 11000L/h;
Continuation dropping sulfuric acid to terminal pH value is 3;
After completion of the reaction, the speed of stirring rake is reduced to 250r/min, 60 DEG C of constant temperature, ageing 1.5 hours;
Washing, dry, pulverizing.
Obtained beer silica gel is carried out opening size test, pore volume test, specific surface area and absorption property test, test result is listed in the table below.
Embodiment 3
10m is added in container
3water as end liquid, be placed in water-bath and be heated to 60 DEG C, then in reactor, add appropriate glycerine 300kg, constant temperature stir 10min;
Get the mixed solution of the above-mentioned water of 1000L and glycerine, stirring velocity is set as 200r/min, dripping volumetric molar concentration toward reactor is the sodium silicate solution of 1mol/L, the pH value of reaction solution is adjusted to 9, and then to add volumetric molar concentration be the sodium silicate solution of 1mol/L and volumetric molar concentration is simultaneously the sulphuric acid soln of 4.2mol/L, and continues to drip sodium silicate solution, control process pH value is 8 ~ 10, the total addition level of sodium silicate solution is 1000L, adds complete, and the interpolation speed of sodium silicate solution is 9000L/h;
Continuation dropping sulfuric acid to terminal pH value is 2;
After completion of the reaction, the speed of stirring rake is reduced to 250r/min, 60 DEG C of constant temperature, ageing 1.5 hours;
Washing, dry, pulverizing.
Obtained beer silica gel is carried out opening size test, pore volume test, specific surface area and absorption property test, test result is listed in the table below.
Embodiment 4
10m is added in container
3water as end liquid, be placed in water-bath and be heated to 60 DEG C, then in reactor, add appropriate glycerine 400kg, constant temperature stir 10min;
Get the mixed solution of the above-mentioned water of 1000L and glycerine, dripping volumetric molar concentration toward reactor is the sodium silicate solution of 1mol/L, the pH value of reaction solution is adjusted to 8, then to add volumetric molar concentration be the sodium silicate solution of 1mol/L and volumetric molar concentration is simultaneously the sulphuric acid soln of 4mol/L, and continue to drip sodium silicate solution, control process pH value is 8 ~ 10, and the total addition level of sodium silicate solution is 1000L, add complete, the interpolation speed of sodium silicate solution is 9000L/h;
Continuation dropping sulfuric acid to terminal pH value is 2.5;
After completion of the reaction, the speed of stirring rake is reduced to 250r/min, 60 DEG C of constant temperature, ageing 1.5 hours;
Washing, dry, pulverizing.
Obtained beer silica gel is carried out opening size test, pore volume test, specific surface area and absorption property test, test result is listed in the table below.
Comparative example 1 and comparative example 2
Purchasing two kinds of beer silica gels on the market, carry out opening size test, pore volume test, specific surface area and absorption property test respectively to it, test result is listed in the table below.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (5)
1. a preparation method for beer silica gel, its step comprises:
1) mixed with water by glycerine, the mass ratio of glycerine and water is 1:(20-200);
2) step 1 is got) glycerine of gained and the mixed solution V of water
1l, under the condition stirred, add sodium silicate solution, the volumetric molar concentration of described sodium silicate solution is 1.0-1.2mol/L, the pH of mixed solution is transferred to 8-10, and add water glass and sulphuric acid soln, the volumetric molar concentration of described sulphuric acid soln is 4-4.2mol/L, keep the pH of mixed solution at 8-10, when sodium silicate solution adds V altogether
2l, wherein V
1=V
2;
3) continuation interpolation sulphuric acid soln is 2-3 to the pH of mixed solution;
4) stir, then ageing;
5) wash, dry, then pulverize and obtain beer silica gel.
2. the method for claim 1, is characterized in that described step 1) be specially: water is heated to 60-80 DEG C, then is added to the water by glycerine, constant temperature stirs 5-10 minute.
3. method as claimed in claim 2, is characterized in that described step 2) agitation condition specifically: the rotating speed of stirring rake is 200-500r/min.
4. the method for claim 1, is characterized in that: described step 4) be specially, stir 1.5 hours under the constant temperature of 60-90 DEG C, the rotating speed 200-250r/min of stirring rake.
5. the method as described in any one of claim 1-4, is characterized in that: described step 2) the interpolation speed of mesosilicic acid sodium is 6000-11000L/h.
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| CN104258806B (en) * | 2014-09-25 | 2017-06-27 | 刘主良 | The preparation method of Bio-sil air purifying particles |
| CN112047352B (en) * | 2019-07-08 | 2021-11-30 | 福建远翔新材料股份有限公司 | Production method of silicon dioxide for beer anti-clouding agent with high adsorption efficiency |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103043670A (en) * | 2012-12-26 | 2013-04-17 | 青岛中能集团有限公司 | Process flow of novel water-absorbent silica gel |
| CN103159220A (en) * | 2011-12-15 | 2013-06-19 | 中国石油天然气股份有限公司 | Method for preparing macroporous silica gel |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103159220A (en) * | 2011-12-15 | 2013-06-19 | 中国石油天然气股份有限公司 | Method for preparing macroporous silica gel |
| CN103043670A (en) * | 2012-12-26 | 2013-04-17 | 青岛中能集团有限公司 | Process flow of novel water-absorbent silica gel |
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Address after: 526238 No. 23 Yingbin Road, national hi tech Industrial Development Zone, Guangdong, Zhaoqing Applicant after: ZHAOQING JINSANJIANG SILICON MATERIALS CO., LTD. Address before: 526238 No. 23 Yingbin Road, national hi tech Industrial Development Zone, Guangdong, Zhaoqing Applicant before: Zhaoqing Jinsanjiang Chemical Co., Ltd. |
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Address after: 526238 No. 23 Yingbin Road, national hi tech Industrial Development Zone, Guangdong, Zhaoqing Patentee after: Jinsanjiang (Zhaoqing) silicon material Co., Ltd Address before: 526238 No. 23 Yingbin Road, national hi tech Industrial Development Zone, Guangdong, Zhaoqing Patentee before: Zhaoqing Jinsanjiang Silicon Material Co., Ltd. |