CN1017778B - Preparation of filter aid from diatomite - Google Patents
Preparation of filter aid from diatomiteInfo
- Publication number
- CN1017778B CN1017778B CN 88109070 CN88109070A CN1017778B CN 1017778 B CN1017778 B CN 1017778B CN 88109070 CN88109070 CN 88109070 CN 88109070 A CN88109070 A CN 88109070A CN 1017778 B CN1017778 B CN 1017778B
- Authority
- CN
- China
- Prior art keywords
- diatomite
- roasting
- filter aid
- pulverizing
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
Abstract
The present invention relates to a method for preparing a beer filter aid from diatomite, wherein the content of SiO2 of the diatomite is from 75 to 85%. The method comprises the following steps: diatomite is crushed, acidized, purified, washed, dried, added with fluxing agents, mixed, calcined, crushed, treated for surface activity and activated at low temperature, and two kinds of filter aids of a burning product for filtering and a fusing agent burning product suitable for beer production can be obtained. The content of Fe3O3 of the diatomite is less than 0.7%, and thus, the quality of the diatomite is stable. Compared with internal and external products of the same kind, the method has the advantages of fast filtering rate, low product consumption, high clarity and low price, and can satisfy the requirements of filtration technologies of beer production.
Description
The invention relates to utilize and contain SiO
275～85% diatomite prepare the method for beer filtering-aid agent.
The well-known height of producing the used filter aid iron-holder of beer.Color to beer can change.Make iron taste on the beer band, also can cause the beer spewing phenomenon.Therefore, the general employing of domestic production beer filtering-aid agent contains SiO
2More than 90%, contain Fe
2O
3At the smart soil of the diatomite below 1.5%.But, cost is raise because smart native reserve is limited.Moreover smart soil is not directly used in the production filter aid by purification processes.Its difficult quality guarantee, thereby can not satisfy the needs of Beer Brewage.The method that adopts diatomite to produce filter aid both at home and abroad is at present: economize extraction → fragmentation → oven dry → grinding → purification → batching → roasting → cooling → grinding → technologies such as screening → finished product packing that Li Wengaisi Meng Da factory all adopts diatomite original soil as French A Erdaishi province Sheng Baozhi factory and Kang Taer.But the filter aid iron-holder height that this method is produced.And it is big to be used for Beer Brewage consumption filter aid amount, and the rate of filtration is slow." light science and technology communication " (1983～1984 years) bound volume P14～15 report: the production technology of Gansu Province's light industry Research Institute super-cell is: baking powder, crushing, cyclonic separation, add cosolvent, mixing, calcining, crushing, classification and sieve.But this method adopts and contains SiO
2More than 90%, iron content is at the smart soil of the diatomite below 1.3%, thereby the production cost height, owing to do not have removal of impurities, filter aid quality instability.And be used for Beer Brewage, and consumption filter aid amount is big, and the rate of filtration is slow, can not satisfy the beer filtration technological requirement.Therefore Beer Brewage producer wishes urgently that all production is a kind of cheap, steady quality, and iron-holder is low, and the rate of filtration is fast, the filter aid that consumption is low.
Method proposed by the invention exactly in order to overcome above-mentioned deficiency, and is produced the method that a kind of new low-grade diatomite of usefulness prepares beer filtering-aid agent.
Method proposed by the invention is: utilize its chemical analysis of low-grade diatomite to be SiO
275～85%, Al
2O
3≤ 7.0%, Fe
2O
3≤ 4.0%, bright mistake≤7.0%.Through pulverizing, acidification, washing, dry, add flux batching, calcining, surface-active-treatment, low-temperature activation and promptly obtain the beer filtering-aid agent that adopts the inventive method to prepare.
According to method proposed by the invention: the pulverizing of being said here is meant pulverizes a diatomite original soil that contains top described component, carries out in order to the preparation of back.Here said acidification.Be that original soil is purified.Because water elutration method, calcination method and pneumatic concentration are generally adopted in traditional purification.But these methods all can not fundamentally be removed the impurity in the diatomite micropore.Especially inapplicable especially to the high diatomite of impurity content.Therefore, acidification proposed by the invention just can effectively be removed Fe
2O
3, Al
2O
3, impurity such as CaO, MgO.Here said acidulant is meant hydrochloric acid, sulfuric acid, and its concentration is 4～30%.Concentration is hanged down has influenced removing of impurity.The concentration height can make preparation cost raise.Preferably adopt 5～15% hydrochloric acid.Original soil mud after acidifying washs with filter press, washing agent is 30～60 ℃ a hot water, with soluble chloride and free acid in the flush away mud, be washed till pH value of filtrate and be till 6～7, again the slurry filter-cake after washing is put into drying shed and carry out drying, adopting baking temperature is 90～150 ℃, and diatomite after drying is because particle is too thin, most of less than 20 μ, be used for filtered beer and can make the rate of filtration slow.Therefore, must process processing, adapt to the needs of beer filtration, for reaching this purpose to change size distribution, particle structure and surface nature.The present inventor has proposed the adding cosolvent, by calcining the method for back change particle structure.As having of this class cosolvent: K
2CO
3, KOH, NaOH, Na
2CO
3, NaCl and alkaline metal salt.Because the Fe ion is easy and the Cl ion combination generates FeCl
3And evaporate, and make filter aid become loose.The present inventor proposes to add chloride and changes particle structure and remove impurity iron, addition 3～20%.Cosolvent is mixed in the dried diatomite of purifying, after mixing, places the high temperature kiln roasting, sintering temperature is 800～1100 ℃.Roasting time is 1～3 hour, cool to room temperature then, through pulverizing 150 orders, be and burn till the product filter aid, the requirement of crossing according to beer, the present inventor has proposed to burn till the activated again preparation method of product filter aid, promptly handle through active surface again burning till the product filter aid, because the filter aid surface texture after roasting is pulverized can not satisfy the needs of Beer Brewage, influenced the rate of filtration of filtered beer, so must carry out surface activation process, as having of this class activator: acetic acid, citric acid, phosphoric acid etc.Its working concentration is 1～10%, be preferably 1～5%, also available water activates, and under condition of stirring, solvent is burnt till product put into the solution that contains surfactant, after treating dispersed with stirring, its solution is filtered,, filter cake is put into baking oven carry out low-temperature activation because the filter aid structure behind surface active is still unstable, temperature is low, and activating velocity is slow; High easy caking is 80～140 ℃ so generally adopt activation temperature, and soak time is 10～26 hours, just obtains the said solvent of the present invention and burns till product.
According to preparation method proposed by the invention, the super-cell iron-holder of preparing is low, and constant product quality is used for beer filtration, can accelerate beer filtration speed, and the filter aid consumption is low, has reduced beer production cost.Simultaneously also can utilize low-grade diatomite, develop low-grade diatomaceous new purposes, reduce the production cost of filter aid, satisfy the needs of Beer Brewage as raw material.Also can be used for industries such as syrup, liquor, beverage, chemical industry, oil.
The preparation of embodiment 1 smart soil
A. get diatomite original soil and (contain SiO for 1 kilogram
282.91%.Fe
2O
32.22%.Al
2O
35.4%, MgO0.97%, CaO0.66% burns and loses 7.55%).Put into beaker, adding concentration is 8% HCl2.4 liter, and stir on the limit, the limit heating, when temperature rises to 90 ℃, constant temperature 3 hours, and simultaneously continuous supplementing water, its amount of makeup water is consistent with the water evaporates amount, carries out vacuum cleaning with Buchner funnel then, is that 50 ℃ hot water washs with temperature.Make the pH value of cleaning solution reach at 6.5 o'clock and get final product, pour filter cake into basin again.Put into baking oven in 100 ℃ dry 24 hours down, promptly obtain the smart soil of diatomite (calling smart soil in the following text) through purifying.
B. other method is identical with A with consumption.Removing used HCl concentration is 3%.
Analyze with chemical method.Its result such as table 1.
Embodiment 2, and flux burns till the preparation of product
A. get K
2CO
370g, NaCl40g puts into beaker, adds 250ml water, puts into smart native 1kg after dissolving.After mixing, put in the evaporating dish, place in the muffle furnace and calcine, when temperature rose to 980 ℃, constant temperature was cooled to room temperature in 1.5 hours, took out the back and pulverized.Cross 150 mesh sieves, put into beaker again, add and contain 4 liters of 5% aqueous citric acid solutions.After dispersed with stirring is even, pour vacuum filtration in the funnel into, again filter cake is put into baking oven.Activate 24 hours down at 140 ℃, promptly obtain sample 1.
B. other preparation method is identical with A with consumption.Except that the KOH that adds is that 40g and KCL are the 20g, just obtain sample 2.
C. except that not carrying out surface activation process and the low-temperature activation.All the other methods and composition are identical with A, just obtain sample 3.
Embodiment 3. burns till the preparation of product
A. get smart native 1kg, put into beaker, Na
2CO
320g puts into another beaker.After adding 200 milliliters of in-depths of water, pour into mix in the smart native beaker after, in the evaporating dish of packing into then, put into muffle furnace and calcine, be warmed up to 900 ℃ after, constant temperature 3 hours is cooled to room temperature.Cross 500 mesh sieves and just obtain sample 4.
B. other is identical with A, but does not add Na
2CO
3, just obtain sample 5.
With chemical analysis and physics method for measuring sample 1～4 is carried out composition and physico-chemical property mensuration.And compare with product of the same type that the U.S. and France produce, it the results are shown in the table II.
Annotate: S is West Germany's product, and J is U.S.'s product, and CBL is the method home made article.A is that thick product is similar to sample 1,2; B is that thin product is similar to sample 4 with CBL.
By the table II as seen, adopt the filter aid of the inventive method preparation, contain SiO
2Height, Fe
2O
3Content be starkly lower than the content of similar products at home and abroad.
Application examples 1
The detection method of the rate of filtration is: in the laboratory, be the 400mm mercury column with vacuum.The filtration effective area is 446.7mm
2, room temperature, filter aid device are 10g.Filter medium is a distilled water.With this understanding, every filtration finishes the required time of 100 ml distilled waters, is the rate of filtration second of filter aid.Sample 1～4 is put into filter measure, it the results are shown in the table III.
By the table III as seen, adopt the prepared filter aid of method proposed by the invention.The content of cosolvent is directly proportional with the rate of filtration in the filter aid, and the activated filter aid rate of filtration is faster than the not activated filter aid rate of filtration.
Comparative example 1
Under laboratory condition, be the 400mm mercury column promptly in vacuum, filter area 446.7mm
2Condition under, compare mensuration with the Hyfto Super-Cel product of sample 1 and U.S. Jones Manville Corp. (US) Patent Department P.O. Box 5108 Denver, Colorado 80217-5108, filter 500 ml distilled waters or beer altogether, divide 5 filtrations, each 100 milliliters.It the results are shown in the table VI.
By the table VI as can be known, the filter aid that method proposed by the invention is prepared is compared with U.S. product of the same type, has that the rate of filtration is fast, turbidity is low, thereby has reduced the consumption of filter aid in the Beer Brewage, has improved the transparency of beer.
Table 1
Composition % SiO
2Fe
2O
3Al
2O
3CaO MgO burns and loses
Title
Smart native A 88.87 0.46 3.93 0.21 0.49 5.2
Smart native B 85.1 1.078 4.8 0.48 0.62 7.8
The table II
Sample SiO
2Fe
2O
3Al
2O
3CaO MgO dehydration part bulk density true specific gravity of burning
Title (g/ml) (g/ml)
Sample 1 94.40 0.40 1.67 0.32 0.43 0.56 0.21 0.36 2.27
Sample 2 87.13 0.61 5.28 0.31 0.91 0.60 0.05 0.34 2.77
Sample 4 94.39 0.53 1.84 0.73 0.53 1.16 0.83 0.33 2.08
Wide A-S 87.15 1.22 4.05 1.37 1.46 0.88 0.11 0.366-
Wide A-J 85.73 1.46 3.77 1.47 0.58 0.25 0.12 0.316 2.27
Wide B-J 92.65 0.83 2.56 1.10 0.43 0.14 0.35 0.30 2.38
CBL 88.93 2.90 4.67 1.31 0.88 0.65 0.21 0.26 2.27
The table III
Sample adds the dosage rate of filtration of fluxing
Sample 1 11 20～29
Sample 20 68～92
Sample 3 11 41～50
Sample 42 165～178
Sample 50 710～785
The table VI
Volume sample 1 U.S. Hyfto Super-Ca
Order distilled water beer distilled water beer
Turbidity time time time time turbidity
First 100 26 " 31 ' 43 " 1-45 " 43 ' 12 " 6-
Second 100 26 " 92 ' 17 " 6-44 " 74 ' 0 "-
The 3rd 100 26 " 02 ' 48 " 0 0.5 44 " 15 ' 3 " 0 1.0
The 4th 100 27 " 03 ' 33 " 5＜10 43 " 75 ' 43 " 2
The 5th 100 26 " 94 ' 14 " 1 0.5 6 ' 17 " 2.0
Claims (3)
1, a kind ofly prepares the method for filter aid, it is characterized in that containing SiO with diatomite
2Amount be 75～85% diatomite through pulverizing, acidifying, washing, oven dry after, add cosolvent again and mix, roasting then, pulverizing, active surface are handled, low-temperature activation just obtains the said filter aid of the present invention, its technical characterictic is:
It is containing SiO that diatomite is pulverized
2Amount is that 75～85% diatomite is crossed 80 mesh sieves through pulverizing the back all-pass;
Acidifying is to be 1～3 to put in the enamel reaction still being 5～15% hydrochloric acid solution through the diatomite after pulverizing and content by solid-to-liquid ratio, is heated to 80～120 ℃, constant temperature 1～4 hour;
Washing is that the diatomite after the acidified processing is separated with centrifuge or sheet frame limit filter with oven dry, removes solution, washs with 30～60 ℃ warm water again, washs cleaning solution pH value and is till 6～7.Separate with centrifuge then, the diatomite after the washing is dry under 90～120 ℃ of temperature, and constant temperature 5～10 hours makes its moisture less than till 5%;
It is flux to be joined in after drying the diatomite mix that flux mixes, and its addition is 3～20% (in dried diatomite);
Roasting is that the diatomite that adds after flux mixes is put into the roasting kiln roasting, and its temperature is 800～1100 ℃, and roasting time is 1～3 hour;
Pulverizing and active surface processing are that the diatomite (semi-finished product) after the process roasting is pulverized, and require 95% by 150 mesh sieves, put into then in the blender, and the adding surfactant, its addition is that the diatomaceous weight ratio after pulverizing with roasting is 1: 0.5;
Low-temperature activation is that the diatomite after the process activation processing is separated unnecessary activating agent with centrifuge, puts into then in the drier, and under 80～140 ℃ of temperature, soak time is 10～26 hours, just obtains filter aid proposed by the invention;
2,, it is characterized in that the K that has as auxiliary agent according to the said method of claim 1
2CO
3, KOH, NaCl, NaOH, Na
2CO
3And alkali metal salt.
3, according to the said method of claim 1, it is characterized in that need adding surfactant, be 1～10% available water also as have acetic acid, citric acid, phosphoric acid, its concentration of surfactant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88109070 CN1017778B (en) | 1988-09-30 | 1988-09-30 | Preparation of filter aid from diatomite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88109070 CN1017778B (en) | 1988-09-30 | 1988-09-30 | Preparation of filter aid from diatomite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1044233A CN1044233A (en) | 1990-08-01 |
| CN1017778B true CN1017778B (en) | 1992-08-12 |
Family
ID=4835333
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 88109070 Expired CN1017778B (en) | 1988-09-30 | 1988-09-30 | Preparation of filter aid from diatomite |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1017778B (en) |
Families Citing this family (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1048647C (en) * | 1994-02-25 | 2000-01-26 | 黄军梁 | Method for prepn. of filter aid using asbestos tailing |
| US5656568A (en) * | 1995-08-11 | 1997-08-12 | Advanced Minerals Corporation | Highly purified biogenic silica product |
| CN1304104C (en) * | 2004-12-13 | 2007-03-14 | 马菊云 | Regeneration technology for waste residue of diatomaceous earth filter aid of sulphonate production refuse |
| EP2411329B1 (en) | 2009-03-11 | 2021-05-19 | Imerys Filtration Minerals, Inc. | Natural amorphous silica filler products |
| CN102091591A (en) * | 2010-12-29 | 2011-06-15 | 广东工业大学 | Kieselguhr modified adsorption material and preparation method and application thereof |
| CN102343253B (en) * | 2011-08-12 | 2012-08-15 | 江苏赢海美联新材料科技有限公司 | Filtering sorbent material, its preparation method and its application |
| CN103055603B (en) * | 2013-03-02 | 2014-12-24 | 郭涛 | Preparation method of ceramic film organic mineral substance filter aid |
| CN103981752B (en) * | 2014-04-29 | 2016-08-24 | 华南理工大学 | A kind of cation-modified preparation method determining agent of the DCS of being applied to |
| CN104803389A (en) * | 2015-03-27 | 2015-07-29 | 辽宁中远高科有限公司 | Purification method of diatomite |
| CN105582883B (en) * | 2015-12-25 | 2017-12-15 | 北海开元生物科技有限公司 | A kind of activated diatomaceous earth and the application in blood product production |
| CN105582884B (en) * | 2016-01-25 | 2017-12-01 | 临江北峰硅藻土有限公司 | A kind of preparation method of food, pharmaceutical products super-cell |
| CN108905958A (en) * | 2018-07-13 | 2018-11-30 | 临江市长白山助滤剂有限公司 | A kind of preparation method of super-cell |
| CN109603300A (en) * | 2018-12-14 | 2019-04-12 | 临江远通硅藻土新材料有限公司 | The method of low-grade diatomite production low bulk density composite filter aid |
| CN109939646A (en) * | 2019-03-01 | 2019-06-28 | 牟丽慰 | A kind of preparation method of super-cell |
| CN115318244A (en) * | 2022-08-24 | 2022-11-11 | 长白朝鲜族自治县天宝硅藻土功能制品有限公司 | Raw ore filter aid for producing diatom and process preparation method thereof |
-
1988
- 1988-09-30 CN CN 88109070 patent/CN1017778B/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| CN1044233A (en) | 1990-08-01 |
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