CN104014300B - Diatomite preparation is with the method for drainage functional beer stabilizing agent - Google Patents
Diatomite preparation is with the method for drainage functional beer stabilizing agent Download PDFInfo
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- CN104014300B CN104014300B CN201310320439.8A CN201310320439A CN104014300B CN 104014300 B CN104014300 B CN 104014300B CN 201310320439 A CN201310320439 A CN 201310320439A CN 104014300 B CN104014300 B CN 104014300B
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Abstract
The invention discloses the method for a kind of diatomite manufacture with the Beer stabilizer of drainage function, it mainly comprises: select the diatomite of amorphous silica content more than 92% to be raw material, clean through waterpower, high-temperature calcination, diluted acid activates, diluted alkaline neutralizes, the operations such as drying, make the individual fully dispersion of diatom without adhesion, clean surface, hole is clear, amorphous silica content reaches more than 99%, iron ion content is lower than 1ppm, water-soluble metal salt is lower than 100ppm, diatom surface silanol group quantity reaches 3-7/nm2, stronger selective absorption function is had to causing the high molecular weight protein of Formation of Beer Chill Haze, effectively extend the shelf-life of beer, it is the favorable substitutes of Prof. Du Yucang beer silica gel.
Description
Technical field
The present invention relates to a kind of production method extending the Beer stabilizer of beer shelf-life, refer in particular to the method for diatomite preparation with drainage functional beer stabilizing agent.
Background technology
Beer is a kind of LA, is confirmed as one of nutraceutical.China is the first big country of world beer output and consumption figure, nearly 4,000 ten thousand tons of current annual production.The quality of beer is the fundamental of beer producers product competition.The shelf-life of beer is again one of key index weighing beer quality, current beer producers is the main method of the shelf-life extending beer is dose the beer silica gel of Prof. Du Yucang (Beer stabilizer), cause the high molecular weight protein of Formation of Beer Chill Haze in order to absorption, reach the order ground extending beer shelf-life.Domestic enterprise of China produce beer silica gel in product purity, adsorptivity, granularity etc. all lower than the product standard of developed countries.Domestic Beer manufacturing enterprise beer silica gel generally used is all based on imported product, expensive, slow to delivery date.
The high absorption beer silica gel production technology of world advanced person is always by the minority enterprise of U.S., day, De Deng developed country is monopolized.The location of its product is the superfine silica gel powder (containing beer silica gel) of high added value, and its main production process is: 1, with high-purity liquid soluble glass for raw material, inorganic acid neutralization reaction, is settled out amorphous silica; 2, ultra-fine grinding (particle diameter 10 ~ 20um); 3, spraying dry.And domestic beer silica gel production method is substantially identical with overseas enterprise, but product purity, granularity, adsorptivity, etc. in far below external product.
The beer silica gel of Prof. Du Yucang self with having good adsorptivity, but does not have drainage function substantially, and serves certain inhibition to the filtration of beer.With alleviate and offset add beer silica gel after the beer filtration resistance that increases, in beer filtration, need the consumption increasing filter aid, virtually increase the filtration cost of beer.In addition, beer silica gel is all with the high-purity alkaline waterglass of liquid for raw material, problems such as generating through sour neutralization reaction, also exist that product energy consumption is high in production, the production cycle is long, one-time investment is large, input and output rate is low, production cost is high.Therefore research and develop the beer silica gel substitute of high-performance and low-cost, have very important significance.
Therefore research and develop the beer silica gel substitute of high-performance and low-cost, have very important significance.
Summary of the invention
The invention provides the method for a kind of diatomite preparation with drainage functional beer stabilizing agent, to solve, Prof. Du Yucang beer silica gel production cost is high, the production cycle long, product does not have the problems such as drainage function.
The present invention adopts following technical scheme:
Diatomite preparation, with the method for drainage functional beer stabilizing agent, is characterized in that, comprises the following steps:
(1), select the diatomite of amorphous silica content more than 92% to be raw material, fully clean in diatomite waterpower swaging machine, make diatom individual separated from one another without adhesion, and clean surface, hole is clear;
(2) diatomite, after cleaning puts into industrial high temperature kiln, and calcine, to remove the organic matter in diatomite, calcining heat is 400 ~ 900 DEG C, and calcination time is 1 ~ 3 hour;
(3) diatomite, after calcining loads with in the container of anti-corrosion function, by diatomite weight ratio add concentration be 5 ~ 50% inorganic acid carry out acid activation process, processing time is defined as 1 ~ 60 hour according to the type of major impurity in diatomite, the temperature of process is 10 ~ 100 DEG C, inorganic acid used is sulfuric acid, nitric acid, hydrochloric acid, phosphoric acid etc., is about 4.5 with distilled water flushing to PH after acid activation process;
(4), the diatomite that the pH value after acid activation process is about about 4.5 is put into container, reconciling PH with alkali is between 6.5 ~ 7.0, alkali used comprises potassium hydroxide, NaOH, potash and sodium carbonate etc., below 100ppm is less than to soluble-salt again with distilled water flushing, i.e. available general precipitation, the equipment dischargings such as filtration or press filtration.
(5), filtration or press filtration gained filter cake putting into drying machine, being no more than drying under the temperature conditions of 200 DEG C, obtaining the diatomite Beer stabilizer with drainage function.
(6), in the diatomaceous waste water of acid activation process containing inorganic acid, alkali metal or alkali salt neutralisation treatment can be added by calipers method and reach national environmental protection and allow discharge standard to discharge.
From the above-mentioned description to structure of the present invention, compared to the prior art, tool of the present invention has the following advantages:
1, through the diatomite of said method process, amorphous silica content reaches more than 99%, and average grain diameter is about 10um, and soluble iron ion concentration is less than 1ppm, and water-soluble metal salt is less than 100ppm, and diatom surface silanol group quantity is 3-7/nm2.
2, by nonmetallic mineral kieselguhr powder surface functionalization, substitute the beer silica gel of Prof. Du Yucang, production cost obtains and significantly reduces.
3, the porous of diatomite self is not with drainage function (beer silica gel of Prof. Du Yucang has), can reduce the consumption of filter material in using, and reduces the consumption of filter material when beer enterprise filters, reduces filtration cost.
4, found the factory small investment, the construction period is short, and device fabrication is easy, and in production, energy resource consumption is few, and technique is simple, adapts to large-scale industrial production.
5, low emission, pollution-free, in the waste liquid of acid activation process, acid content is low, can reach discharge standard by simple neutralisation treatment, then non-pollutant discharge in other production stage.
Detailed description of the invention
The following describes the specific embodiment of the present invention.
Embodiment 1
(1) take 10kg diatomite, wherein disk algae, melosira respectively account for 50%, put into special diatomite waterpower swaging machine and add water 40 liters and clean 2.5 hours.Sample thief basis of microscopic observation, without adhesion between diatom, become the individual shape of dispersion, diatom clean surface, hole is clear.Slurry is entered in sedimentation basin, after diatomite precipitation, discharges supernatant liquid, take out diatomite aqueous deposit.
(2) diatomite aqueous deposit is put into industrial oven, dry at 200 DEG C of industrial temperature.Diatomite after drying is loaded in ceramic saggar and puts into industrial electric furnace, 800 DEG C of temperature lower calcinations 2 hours, as far as possible by clean for the organic burn off in diatomite.
(3) get the diatomite 5kg after calcining and put into plastic containers, add the aqueous sulfuric acid 30 liters that concentration is 5%, normal temperature activation process 2 hours, middle (about 1 hour) fully stirs once.After 2 hours after diatomite fully precipitates, discharge upper strata waste liquid, add distilled water stirring precipitation, this process is several repeatedly, until take out the diatomite through abundant precipitation when aqueous ph value reaches 4.5.
(4) diatomite being 4.5 the pH value after diluted acid activation loads in common container, add 30 liters of distilled water simultaneously, repeatedly clean with distilled water after regulating pH value to 6.5 with NaOH, until water soluble salt is low to below 100PPm, i.e. the desirable diatomite of various conventional method such as available precipitation, filtration, press filtration.
(5) the diatomite wet feed taken out is dried to water content by common industrial drying machine temperature below 200 DEG C and is less than 1%, obtain the diatomite Beer stabilizer with drainage function.After testing, noncrystalline SiO
2content is 99.1%, and average grain diameter is about 10um, and water soluble salt is less than 100PPm, and soluble iron ion is less than 1PPm, and diatom surface silanol group is 3 ~ 5/nm2.Detect through certain beer enterprise technique center domestic, its absorption property reaches import beer silica gel level.
Embodiment 2
(1) take 10kg diatomite, wherein disk algae accounts for 80%, melosira accounts for 20%, puts into special diatomite waterpower swaging machine and adds water 40 liters and clean 2 hours.Sample thief basis of microscopic observation, without adhesion between diatom, become the individual shape of dispersion, diatom clean surface, hole is clear.Slurry is entered in sedimentation basin, after diatomite precipitation, discharges supernatant liquid, take out diatomite aqueous deposit.
(2) diatomite aqueous deposit is put into industrial oven, dry at 200 DEG C of industrial temperature.Diatomite after drying is loaded in ceramic saggar and puts into industrial electric furnace, 850 DEG C of temperature lower calcinations 2 hours, as far as possible by clean for the organic burn off in diatomite.
(3) get the diatomite 5kg after calcining and put into plastic containers, add the aqueous hydrochloric acid solution 30 liters that concentration is 5%, normal temperature activation process 2 hours, middle (about 1 hour) fully stirs once.After 2 hours after diatomite fully precipitates, discharge upper strata waste liquid, add distilled water stirring precipitation, this process is several repeatedly, until take out the diatomite through abundant precipitation when aqueous ph value reaches 4.5.
(4) diatomite being 4.5 the pH value after diluted acid activation loads in common container, adds 30 liters of distilled water simultaneously, uses Ca
2cO
3regulate after pH value to 6.5 and repeatedly clean with distilled water, until water soluble salt is low to below 100PPm, i.e. the desirable diatomite of various conventional method such as available precipitation, filtration, press filtration.
(5) the diatomite wet feed taken out is dried to water content by common industrial drying machine temperature below 200 DEG C and is less than 1%, obtain the diatomite Beer stabilizer with drainage function.After testing, noncrystalline SiO
2content is 99.4%, and average grain diameter is about 10um, and water soluble salt is less than 100PPm, and soluble iron ion is less than 1PPm, and diatom surface silanol group is 4 ~ 6/nm2.Detect through certain beer enterprise technique center domestic, its absorption property reaches import beer silica gel level.
Embodiment 3
(1) take 10kg diatomite, wherein disk algae content is greater than 95%, other algae accounts for 5%, puts into special diatomite waterpower swaging machine and adds water 40 liters and clean 1.5 hours.Sample thief basis of microscopic observation, without adhesion between diatom, become the individual shape of dispersion, diatom clean surface, hole is clear.Slurry is entered in sedimentation basin, after diatomite precipitation, discharges supernatant liquid, take out diatomite aqueous deposit.
(2) diatomite aqueous deposit is put into industrial oven, dry at 200 DEG C of industrial temperature.Diatomite after drying is loaded in ceramic saggar and puts into industrial electric furnace, 900 DEG C of temperature lower calcinations 2 hours, as far as possible by clean for the organic burn off in diatomite.
(3) get the diatomite 5kg after calcining and put into plastic containers, add the aqueous solution of nitric acid 30 liters that concentration is 5%, normal temperature activation process 2 hours, middle (about 1 hour) fully stirs once.After 2 hours after diatomite fully precipitates, discharge upper strata waste liquid, add distilled water stirring precipitation, this process is several repeatedly, until take out the diatomite through abundant precipitation when aqueous ph value reaches 4.5.
(4) diatomite being 4.5 the pH value after diluted acid activation loads in common container, adds 30 liters of distilled water simultaneously, uses Ca
2cO
3regulate after pH value to 6.5 and repeatedly clean with distilled water, until water soluble salt is low to below 100PPm, i.e. the desirable diatomite of various conventional method such as available precipitation, filtration, press filtration.
(5) the diatomite wet feed taken out is dried to water content by common industrial drying machine temperature below 200 DEG C and is less than 1%, obtain the diatomite Beer stabilizer with drainage function.After testing, noncrystalline SiO
2content is 99.8%, and average grain diameter is about 10um, and water soluble salt is less than 100PPm, and soluble iron ion is less than 1PPm, and diatom surface silanol group is 5 ~ 7/nm2.Detect through certain beer enterprise technique center domestic, its absorption property reaches import beer silica gel level.
Above are only the specific embodiment of the present invention, but design concept of the present invention is not limited thereto, all changes utilizing this design the present invention to be carried out to unsubstantiality, all should belong to the behavior of invading scope.
Claims (5)
1. diatomite preparation is with the method for drainage functional beer stabilizing agent, it is characterized in that, comprise the following steps: (1), the diatomite of selection amorphous silica content more than 92% are raw material, fully clean in diatomite waterpower swaging machine, make diatom individual separated from one another without adhesion, and clean surface, hole is clear;
(2) diatomite, after cleaning puts into industrial high temperature kiln, and calcine, to remove the organic matter in diatomite, calcining heat is 400 ~ 900 DEG C;
(3), calcining after diatomite load carry out dilute acid pretreatment with in the container of anti-corrosion function, the processing time is 1 ~ 60 hour;
(4), with the diatomite in alkali and after dilute acid pretreatment, and use distilled water to pass through repeatedly to wash the water-soluble metal salt removed in diatomite to reach below 100ppm, i.e. sedimentation and filtration or press filtration discharging;
(5), filtration or press filtration gained filter cake putting into drying machine, being no more than drying under the temperature conditions of 200 DEG C, obtaining the diatomite Beer stabilizer with drainage function.
2. diatomite preparation as claimed in claim 1 is with the method for drainage functional beer stabilizing agent, it is characterized in that: the scouring time described in step (1) is 1 ~ 3 hour.
3. diatomite preparation as claimed in claim 1 is with the method for drainage functional beer stabilizing agent, it is characterized in that: in step (3) dilute acid pretreatment use acid for inorganic acid be sulfuric acid, one in nitric acid, hydrochloric acid and phosphoric acid, the use amount of diluted acid and diatomaceous weight ratio are 5 ~ 50%, and the temperature of dilute acid pretreatment is 10 ~ 100 DEG C.
4. the diatomite preparation as described in claim 1 or 3, with the method for drainage functional beer stabilizing agent, is characterized in that: the waste water after described dilute acid pretreatment adds alkali metal or alkaline-earth metal neutralisation treatment.
5. diatomite preparation as claimed in claim 1 is with the method for drainage functional beer stabilizing agent, it is characterized in that: alkali described in step (4) is the one in potassium hydroxide, NaOH, potash and sodium carbonate, the pH value at the end of the neutralization of this alkali is 6.5 ~ 7.0.
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| CN108264528A (en) * | 2016-12-31 | 2018-07-10 | 烟台大学 | A kind of method that lactose is isolated and purified from whey |
| CN108260800A (en) * | 2016-12-31 | 2018-07-10 | 烟台大学 | The technique for preparing Lactulose liquid using whey |
| 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 (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101224409A (en) * | 2007-10-18 | 2008-07-23 | 烟台博瑞特精细化工有限公司 | Preparing method of aerosol with high adsorption value |
| WO2011144346A1 (en) * | 2010-05-21 | 2011-11-24 | Grace Gmbh & Co. Kg | Porous inorganic oxide particles and methods of making and using the same |
| CN102328933A (en) * | 2011-06-30 | 2012-01-25 | 青岛美高集团有限公司 | Beer silica gel and preparation method thereof |
| CN102527327A (en) * | 2012-02-03 | 2012-07-04 | 昆山市洁驰环保科技发展有限公司 | Method for preparing diatomite serving as filter aid by utilizing rice hulls |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5656568A (en) * | 1995-08-11 | 1997-08-12 | Advanced Minerals Corporation | Highly purified biogenic silica product |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101224409A (en) * | 2007-10-18 | 2008-07-23 | 烟台博瑞特精细化工有限公司 | Preparing method of aerosol with high adsorption value |
| WO2011144346A1 (en) * | 2010-05-21 | 2011-11-24 | Grace Gmbh & Co. Kg | Porous inorganic oxide particles and methods of making and using the same |
| CN102328933A (en) * | 2011-06-30 | 2012-01-25 | 青岛美高集团有限公司 | Beer silica gel and preparation method thereof |
| CN102527327A (en) * | 2012-02-03 | 2012-07-04 | 昆山市洁驰环保科技发展有限公司 | Method for preparing diatomite serving as filter aid by utilizing rice hulls |
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