CN1017777B - Method using low-quality diatomite to process filter aid - Google Patents

Abstract

The present invention relates to a processing technology of a diatomite filter aid and a method for recovering a water purifying agent of aluminium sulphate from waste water drained by the processing technology. The processing technology has the technical flow that the diatomite filter aid is prepared by that raw mine soil is dried, broken, calcined, treated at constant temperature and sulphuric acid addition for reaction, washed in hot water, filtered by pressure, dried, stirred, calcined, treated at constant temperature, washed in hot water, dried, pulverized and sieved, and then, the finished product of the purifying agent is also prepared by that collected waste water is tested, treated by pH value adjustment, concentrated and cooled for crystallization. The technology of the present invention has the advantages of easiness, high quality of the acquired product and good social benefit and economic benefit.

Description

Method using low-quality diatomite to process filter aid

The present invention relates to beverage and filter filter aid and water quality cleansing agent field, particularly with ore deposit inferior original soil process high-quality diatom soil filter aid with and produce after waste water reclaim sulfuric acid aluminium water purifying agent (abbreviation: the method for utilizing grade diatomaceous production filter aid).

Beverage industry (mainly being beer) goes up the filter aid that filters usefulness at present several kinds, and best is the filter aid of processing with diatomite.Diatomite mainly is divided into garden sieve algae and direct-connected algae etc. from its structure, as the diatomite of processing filter aid, requires to contain silica more than 80%, contains diatom greater than 80%, and impurity contents such as alundum (Al and di-iron trioxide are very low.Saying relatively, contain the high more diatomite of silica, is the desirable feedstock as filter aid, and still, the diatomite of this quality whole nation reserves seldom; Ropy diatomite, diatom only account for about 50%, and silica has only about 65%, and alundum (Al is up to 18%, and di-iron trioxide is up to 9%, and this class diatomite is quite abundant at China's reserves.

Purpose of the present invention, for the diatom original soil that makes a large amount of poor qualities is developed, the super-cell that provides a kind of usefulness diatom original soil inferior to be processed into the requisite quality standard reclaims the aluminum sulfate water purification agent with the waste water of producing the back discharging simultaneously.This technological process is simple, and the product quality height that obtains can be changed waste materials into sth. useful again.

Be to implement technological process of the present invention and step explanation below:

Mine original soil (being diatom original soil) → dry to water content 55～20% → fragmentation 6～8 mesh sieve branch → calcination, constant temperature → sulfuric acid reaction → hot wash pressure

Add aluminum dross and sour water add thermal response → accent pH value 2.8～3.2 →

Baume degrees 28～crystallisation by cooling got solid sulphuric acid aluminium in 32 o'clock through concentrating.

The explanation of process flow steps:

1. general mine original soil water content 50～60%, contain earth 20%, do to water content 15～20% through overbaking (solarization), at this moment, diatomite is loose, one bump promptly broken, earth is then opposite with diatomite, because of moisture content reduces, earth is formed tough and tensile walk by former completely mashed shape, with 6～8 purpose shaking screens diatomite and earth is separated;

Through above-mentioned steps with diatomite and earth separately after, also deposit about 30% alundum (Al and di-iron trioxide and other impurity in the diatomite; For further work, earlier with isolated diatomite the 1st time 500～850 degree calcination Celsius, constant temperature 45～150 minutes, this moment, silica was inertia, was not subjected to Temperature Influence during calcination, and impurity such as alundum (Al and di-iron trioxide are because high-temperature calcination, fully oxidation;

3. the silica in the sulfuric acid reaction, diatomite is insoluble to sulfuric acid, vitriolizations such as alundum (Al and di-iron trioxide, and the soil with 1: 2.5～3.5, acid solution carry out reacting in 6～8 hours at 90～120 degree Celsius, and reaction equation is:

Diatomite through reacting is by containing silica 66.23% originally, alundum (Al contains 14.58%, di-iron trioxide contains 5.77%, make dioxide-containing silica reach 94.38%, improve 42.5%, alundum (Al only contains 2.76%, removed 81.06%, di-iron trioxide only contains 0.457%, has removed 92.08%, the quality of chemical analysis all above Japan, the U.S. natural with China EC-101 board super-cell (seeing the back subordinate list for details);

4. hot wash press filtration, for guaranteeing in the above-mentioned sulfuric acid reaction impurity such as alundum (Al and di-iron trioxide to be removed as far as possible, therefore, when the reaction complex acid, be with the soil of butt behind calcination, constant temperature 1 gram and 98% sulfuric acid, 0.68～2 gram proportioning, reaction result, the spent acid press filtration is come out, the acid solution that behind precipitated crystal, leaches, its sulfuric acid is than being 50～70% before the original reaction, use in the time of can making down secondary response, also can be used to the reclaim sulfuric acid aluminium water purifying agent.To exist diatomaceous residual acid also need to be washed till till the pH value 6～7 then with the hot wash of 90 degree Celsius;

5. oven dry, batching stirring, calcination, constant temperature, the quality of super-cell, except that improving diatomaceous silica as far as possible, the calcination of also need preparing burden, make the meticulous or particles suspended of diatomite, screen by required grain size category requirement, at this moment, at first will wash good smart soil after 112～200 degree oven dry Celsius, add natrium carbonicum calcinatum and make cosolvent, add sodium chloride as aerating agent, the effect of sodium chloride also is to make aluminium oxide, iron oxide and titanium dioxide silicochromium to close, thereby improves the inherent quality of filter aid.Because super-cell slightly, carefully is speed and the clarity that directly has influence on filtration, for this reason, must do the processing of size distribution to super-cell, the present invention, mainly contain two kinds by the size distribution of filter aid: a kind of is that 150 orders (meal) add 5～10% natrium carbonicum calcinatum and 5～6% sodium chloride; A kind of is that 200 orders (fine powder) add 1～5% natrium carbonicum calcinatum and 1～4% sodium chloride, and two kinds of filter aids are all wanted the 2nd calcination in 850～1100 degree Celsius, constant temperature 1～2 hour;

6. hot wash, owing to added natrium carbonicum calcinatum and sodium chloride alkaline matter in calcination, the product meta-alkalescence so also need use hot wash after calcination, makes the pH value be controlled at (the pH value that refers to filtered beer) about 7;

7. when filtration contained the suspension of fine particle or gelatinous precipitate, other filter mediums were blocked easily, used super-cell of the present invention, can prevent to stop up, and helped to filter to carry out smoothly, and the removal of impurity is good.Before filtering by real requirement earlier with 17% meal, 20% fine powder is coated on the filter in advance, remaining 63%, be added in equably with 0.5～3 kilogram deal and be filtered in the material by the material that is filtered per ton;

8. collect the waste water of this technological process discharging, the test pH value also need add aluminum dross and waste acid water and add thermal response at 90～100 degree Celsius as below 2.5, pH value is transferred to can discharge storage tank at 2.8～3.2 o'clock;

9. concentrate, measuring Baume degrees is 20～22 o'clock, has become liquid aluminium sulfate, and being concentrated to Baume degrees is 28～32 o'clock, can put pan tank into, and crystallisation by cooling just gets solid sulphuric acid aluminium.

Super-cell of the present invention is on probation through Nanning City brewery, / 1000 liters of super-cell addition 0.5～3 grams, respectively champagne and beer are filtered Xian Tu meal-fine powder-meal, every layer of super-cell 10 gram, bottom is that gauze (because of without filter) filters twice, 3 minutes/1000 milliliters of the rates of filtration, do contrast test with cottonseed cake, the no matter rate of filtration and effect, cottonseed cake filters and all is not so good as super-cell of the present invention.

By " Guangxi Medical College's labour health toxicology group is done this super-cell acute toxicity testing ", think that it is safe that this super-cell is used for beer filtration.

Super-cell of the present invention with Japan, the U.S. is natural and quality comparison sheet chemical analysis such as China EC-101 board super-cell (table back note):

Place of production day, Chinese the present invention liked in the U.S.

Composition Ben Dahe state EC-101 board filter aid

Silica 87.90% 89.82% 90.1% 94.38%

Alundum (Al 5.9% 1.82% 4.15% 2.76%

Di-iron trioxide 1.1% 0.44% 0.95% 0.457%

Annotate: the filtration of beverage " beer ", it is high more that super-cell contains silica relatively, filter effect is good more, what hinder the rate of filtration mainly is alundum (Al and di-iron trioxide, ferric oxide content is high more simultaneously, can become redness during filter beverages, so make comparisons with silica, alundum (Al, di-iron trioxide in the table.

Claims (2)

1, a kind of method of utilizing grade diatomaceous filter aid, it is characterized in that utilizing grade diatomaceous (mine original soil) to be raw material, by the mine original soil is dried, pulverize, 500 ℃～850 ℃ calcination, constant temperature 45～150 minutes, mud acid with butt soil 1: 2.5～3.5 carries out 6～8 hours sulfuric acid reactions than at 90 ℃～120 ℃, again with of the ratio complex acid reaction of butt soil 1 gram with 98% sulfuric acid 0.68～2 gram, hot wash PH to 6～7 with 90 ℃, 112 ℃～200 ℃ oven dry, add natrium carbonicum calcinatum and sodium chloride, 850 ℃～1100 ℃ calcination, constant temperature 1～2 hour, the products obtained therefrom hot wash, control PH promptly gets the super-cell finished product about 7.

2, a kind of method of utilizing grade diatomaceous production aluminum sulfate water purification agent, it is characterized in that collecting the waste water that claim 1 is produced filter aid, PH is below 2.5 in test, add aluminum dross and waste acid water, add thermal response at 90 ℃～100 ℃, PH is transferred to 2.8～3.2 aluminum sulfate concentrate, measure Baume degrees 28～32, crystallisation by cooling promptly gets the aluminum sulfate water purification agent.