CN103602808B - The Biological desiliconization method of vanadium titano-magnetite - Google Patents
The Biological desiliconization method of vanadium titano-magnetite Download PDFInfo
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Abstract
The invention belongs to field of ore extraction, the biological desiliconization relating to a kind of vanadium titano-magnetite, with the method for enriched iron, titanium valuable element, is specifically related to the cultivation of silicate bacteria and the treatment process of mineral.The present inventor is in order to realize the biological desiliconization of vanadium titano-magnetite, silicate bacteria is obtained from commercial undertaking, utilize v-ti magnetite breeze to mix Alexandria sieve husband substratum to cultivate it, the silicate bacteria after cultivation is more conducive to the silicon removed in vanadium titano-magnetite.Step is as follows: A, cultivation silicate bacteria: B, pulverizing vanadium titano-magnetite are to crossing 40-400 mesh sieve; C, biological desiliconization.Silicate bacteria is still comparatively obvious to the immersion Zn of silicon in vanadium titano-magnetite.
Description
Technical field
The invention belongs to field of ore extraction, the biological desiliconization relating to a kind of vanadium titano-magnetite, with the method for enriched iron, titanium valuable element, is specifically related to the cultivation of silicate bacteria and the treatment process of mineral.
Background technology
China's Panxi Diqu contains the vanadium titano-magnetite having rich reserves.Its Gold in Ores belongs to mineral and mainly contains ilmenite, titanomagnetite, magnesium-aluminium spinel and a small amount of sulfide, and gangue mineral then mainly silicates mineral, also containing a small amount of phosphoric acid salt and carbonate minerals.With regard to its composition, its total iron content is 23.65 ~ 34.88%, is the composition that content in ore is maximum, is secondly SiO
2(18.18 ~ 29.47%), the less main component of other content comprises CaO (5.15 ~ 8.19%), TiO
2(9.12 ~ 12.03%), Al
2o
3(8.04 ~ 9.62%), MgO (5.61 ~ 6.77%).As can be seen here, in vanadium titano-magnetite, silicon mine is a kind of main component forming vanadium titano-magnetite ore matrix, and its content exists considerable influence to iron in ore, titanium grade.If silicon mine in ore can be made to be destroyed, be no matter the raising (rich long-pending) for iron in ore, titanium grade or follow-up possible beneficiation flowsheet, all can embody favourable effect.In soil, there is the Gram-negative genus bacillus that a class is special in a large number, it can decompose the rock forming mineral be made up of silicate and aluminosilicate and the element such as silicon, potassium, iron that can discharge wherein, and this bacterioid is just referred to as silicate bacteria.Because it is to the effect of ore mesosilicic acid saline minerals, this bacterioid has been widely used in the production of bacterial manure, and the research also mushroom development in process mineral wealth, this respect then mainly concentrates on the desiliconization process of high-silica diaspore ore.
At present, the research work of external this respect report more, domestic rarely seen report.USSR (Union of Soviet Socialist Republics) Kazakhstan carried out kaolinite and gibbsite bioleaching separating experiment, bacillus colloid bacterioid is adopted to leach thin mud and magnetic product, extraction temperature 28 ~ 30 DEG C, liquid-solid ratio is 5, leaches and within 9 days, obtains the desiliconization rate of about 62% and the aluminium recovery of 99%.The research of the people such as Groudeva shows, utilizes the Bacillus circulans of wild and Laboratory Acclimation and the slovenly mutant bacterial classification of mucus bar, leaches silicon, leached the wherein silicon of 73.6% in 5 days from different bauxite.In the bauxite utilizing different sorts silicate bacteria leaching gibbsite type, leach silicon it is still further preferred that B.circulans, it is at pH=5.5-6.0, during 30-35 DEG C, in soluble solids, the content of silicon is 10-15%, shaking flask slewing rate remains on 300-400r/min, and aluminium content can rise to 63.9% from 43.4%, and silicon-dioxide drops to 9.1% from 25%.With the bauxite B.circulans process of the gibbsite type of magnetic separation and flotation, optionally should not dissolve Al
2o
3.SiO
2.2H
2o, and make the aluminum concentration in solution be raised to 6.7%; In concentrated solution, the percentage extraction of aluminium reaches 93.6%.Andreev etc. also have similar report, will containing Al
2o
338.5%, SiO
235 ~ 38%, FeO1.35%, Fe
2o
32.3%, P
2o
50.3%, the manosil AS salt mine of CaO0.6% etc. is through silicate bacteria process, and in leaching slag, aluminium brings up to 46.9%, SiO
2reduce to 19.0%.With silicate bacteria B.mucilaginosus process bauxite, add 20%HCl process, bauxite is (containing Fe
2o
3fe 1.5%-7.0%)
2o
3residual quantity reduces to 1.2%.This bauxite is used to refractory industry.
Sun De fourth class people was once separated the colloid bacillus cereus obtaining 3 strain different sourcess, after domestication is cultivated, carried out desiliconization research to several alum clay sample ore.Result shows, they all can leach the aluminium in aluminium silicate mineral preferably, and leaching yield is at 25.7-65.7%.Dissimilar silicate minerals is different for its crystalline network, and the degree of Bioleaching wherein silicon is different.Bacterium is not so good as obvious to the leaching effect of the silicate minerals of the laminate structure such as chlorite, kaolinite to the leaching effect of the silicate minerals of the rack-like structures such as quartz, feldspar.Utilize the bacterium taming cultivation in the sucrose containing immersed sample ore in advance, and have the leaching carrying out silicon in sugared medium substratum.Its ability leaching silicon obviously more unacclimated bacterial classification or domesticated strain but to carry out the leaching ability of silicon in sugar-free media strong.Adopt Continuous leaching process, the effect of Bioleaching silicon obviously will be better than independent shaking flask leaching effect.Meanwhile, Continuous leaching process can shorten the Bioleaching time (shortening 2-5 days) of sample ore greatly, and the A/S of bauxite raw ore brings up to 11.73 from 3.73.When main gangue mineral in bauxite be kaolinite or chlorite time, its alumina silica ratio can bring up to about 18 from 3.73, and desiliconization rate can reach 82%.
Summary of the invention
The present inventor is in order to realize the biological desiliconization of vanadium titano-magnetite, silicate bacteria is obtained from commercial undertaking, utilize v-ti magnetite breeze to mix Alexandria sieve husband substratum to cultivate it, the silicate bacteria after cultivation is more conducive to the silicon removed in vanadium titano-magnetite.
The biological desiliconization enriching method of vanadium titano-magnetite of the present invention, comprises the steps:
A, cultivation silicate bacteria:
1) silicate bacteria is got, silicate bacteria preferred gums bacillus powder;
Wherein, bacterial classification source is concentrate microbial function yeast (agricultural type) the colloid bacillus powder of Rui Gu bio tech ltd, Baoding.
2) substratum is prepared: the component containing following weight proportioning:
Every 1000ml distilled water adds 4-6g glucide, and 0.25-0.78g(is in P) water-soluble phosphorus containg substances, 30-70mg(is in Mg) magnesium salts, 1-2.8mg(is in Fe) molysite, 32-65mg(is in Ca) calcium salt, 0.5-10g vanadium titano-magnetite, 10-20g jelling agent; Control ph 7-8;
3) silicate bacteria add water make concentration be 0.1% ~ 0.0001% bacteria suspension be placed in step 2) gained substratum cultivates, and obtains the silicate bacteria after cultivating; Wherein, bacteria suspension is added in following ratio: substratum 50g adds 0.1-2ml bacteria suspension and cultivates; The add-on of bacteria suspension does not flow with confluent culture base and is advisable.
The bacterium colony that final substratum generates is intensive, and form, color, gloss are completely the same, does not have other non-silicate bacterial colony.
B, pulverizing vanadium titano-magnetite are to crossing 40-400 mesh sieve; Varigrained ore pulp obtains different silicon leaching effects.Granularity is thinner, and its silicon leaching effect is better.
C, biological desiliconization:
1) preparation biological leaching silicon ore pulp: the component containing following weight proportioning:
Add 3-5.2g glucide in every 1000mL water, 0.43-1.03g(is in P) water-soluble phosphorus containg substances, 1-50mg(is in Mg) magnesium salts, and 0.34-3.44mg(is in Fe) molysite, 4-60mg(is in Ca) and calcium salt, 8-100g vanadium titano-magnetite; Control ph 7-8;
2) desiliconization is cultivated: the silicate bacteria after the cultivation of steps A gained adds in biological leaching silicon ore pulp, and temperature controls at 20-40 DEG C, and cultivate 5-15 days, vanadium titano-magnetite separates out Dissolved Silicon to solution, and solid-liquid separation gets final product desiliconization;
Or
1) prepare silicate bacteria pre-fermentation broth, the silicate bacteria after inoculation step A cultivates, temperature controls at 25-35 DEG C, cultivates 7-14 days, obtains fermented liquid;
Pre-fermentation broth contains the component of following weight proportioning:
Every 1000ml distilled water adds 4-6g glucide, and 0.52-1.29g(is in P) water-soluble phosphorus containg substances, 9.8-69mg(is in Mg) magnesium salts, and 1-2.8mg(is in Fe) molysite, 12-64mg(is in Ca) calcium salt; Control ph 7-8;
2) in step 1) gained fermented liquid, add vanadium titano-magnetite, control pulp density 2%-12%, temperature controls at 10-40 DEG C, and cultivate 2-10 days, vanadium titano-magnetite separates out Dissolved Silicon to solution, and solid-liquid separation gets final product desiliconization.
Wherein, steps A jelling agent is agar, gelatin, silica gel, water soluble polyacrylic or water soluble cellulose class.
Wherein, glucide described in step C is sucrose, glucose, fructose or starch.
Wherein, nonnitrogenous in water-soluble phosphorus containg substances described in step C, potassium, magnesium, calcium or iron.
Wherein, water-soluble phosphorus containg substances described in step C is NaH
2pO
4, Na
2hPO
4or acid phosphate zinc.
In the biological desiliconization enriching method of the present invention, the silicate bacteria after cultivation generally adopts deepfreeze to preserve.
During use, the silicate bacteria bacterial classification of deepfreeze can be inoculated rear cultivation to activate bacterial classification in containing the enrich media of vanadium titano-magnetite, incubation time is 24h at least.Then enlarged culturing be can carry out in agar eutrophy ore pulp, bacterial body vigor and quantity improved.
By vanadium titano-magnetite crushing grinding, granularity can cross 40 mesh sieves can reach the object leaching desiliconization, but in order to improve leaching efficiency, contriver selects the less vanadium titano-magnetite of granularity to operate usually, usually controls to cross 40-400 sieve.
The method of biological desiliconization can adopt following two kinds of modes:
One, is mixed with the ore pulp of 1%-15%, adds the nutritive substance required for silicate bacteria growth, carbohydrate, P contained compound, additionally should add the nutritive ingredients such as nitrogen (can promote that row is long, shorten the treatment time) if desired; In ore pulp, add the silicate bacteria after cultivating, constant temperature carries out solid-liquid separation after leaching for some time, and in leach liquor, silicone content significantly improves.
Its two, silicate bacteria is fermented without ore deposit, namely add in pre-fermentation broth make its bacterial body very dense increase after, directly add after vanadium titano-magnetite constant temperature leaches for some time and carry out solid-liquid separation, in leach liquor, silicone content significantly improves.Cultivate owing to having carried out bacterium pre fermentation in advance, therefore after adding vanadium titano-magnetite, the silicon of a great deal of can be leached in the short period of time.
In the substratum of silicate bacteria bacterial classification for the addition of climb western v-ti magnetite breeze have nitrogen or nitrogen-free agar.Be directed to the desiliconization of vanadium titano-magnetite, silicate bacteria grows required carbohydrate fast and comprises glucose, sucrose, starch, the rich Starch Fraction of plant through boiling, as the potato etc. of boiling.
The raw material that present method can process is vanadium titano-magnetite, also comprise by vanadium titano-magnetite be derived containing silicon materials.The concentration of ore pulp can be controlled in 1% ~ 10%; Silicon extraction temperature 10 DEG C ~ 40 DEG C; Jolting rotating speed 100rpm ~ 400rpm; Extraction time 2 ~ 10 days.
When in silicate bacteria is to vanadium titano-magnetite, silicon leaches, silicon is present among liquid phase with dissolved state.The change in concentration 10% ~ 50% of silicon in liquid phase.
Embodiment
Embodiment 1: cultivate silicate bacteria
To go bail for concentrate microbial function yeast (agricultural type) the colloid bacillus powder of Ding Rui paddy bio tech ltd.
By formula: sucrose 5.01g, NaH
2pO
42.04g, MgSO
47H
2o0.50g, FeCl
30.0052g, CaCO
30.12g, vanadium titano-magnetite (crossing 180 mesh sieves) 1.02g, silica gel 15.05g, distilled water 1000mL prepare bacteria culture medium and sterilising treatment.
(1) take bacterium powder 0.1g, pour in 100mL sterilized water, stir 15min, leave standstill 20min, be mixed with the bacteria suspension of 0.1%; (2) with the pipette, extract lmL(1 of sterilizing) in upper strata bacteria suspension, join in 9mL sterilized water and fully vibrate, make the bacteria suspension that weaker concn is 0.01%; (3) join abundant vibration in 9mL sterilized water with sterilizing transfer pipet test tube absorption lmL bacteria suspension from (2) and make the bacteria suspension of 0.001%; (4) from (3), drawing lmL bacteria suspension with sterilizing transfer pipet joins in 9mL sterilized water, and fully the bacteria suspension of 0.0001% is made in vibration.With sterilizing transfer pipet respectively from 0.1%, 0.01%, 0.001%, draw 0.5mL bacteria suspension 0.0001% 4 kind of diluent and move in four 50g culture medium flat plates respectively, left at room temperature 3-5min, then flat board is inverted, be put in after cultivating 2-4 days in the constant incubator of 30 DEG C, select meet silicate bacteria colony characteristics and do not use containing the flat board of abnormal bacterium colony.If there is abnormal bacterium colony, then select the bacterium colony streak culture 2-4 days on solid medium meeting silicate bacteria colony characteristics, the more single bacterium colony of picking repeats line 2-3 time, uses microscopic examination, till bacterium colony without exception simultaneously.
Embodiment 2: the biological desiliconization of agar ore pulp
3% agar ore pulp: sucrose 1.03g, NaH
2pO
40.42g, MgSO
47H
2o0.15g, FeCl
30.0010g, CaCO
30.0255g, vanadium titano-magnetite 6.16g, agar 3.07g, distilled water 200mL, pH7.5.Silicate bacteria after cultivating is inoculated in slant medium, in 30 DEG C of constant incubators, cultivates 24h, pour in the beaker containing 300ml sterile purified water, make bacteria suspension 1; With the pipette, extract 1ml bacteria suspension 1 of sterilizing in containing in the beaker of 100ml sterile purified water, make bacteria suspension 2; With the pipette, extract 2ml bacteria suspension 2 of sterilizing in containing in the beaker of 100ml sterile purified water, make bacteria suspension 3.Draw 1ml bacteria suspension 1 in 3% agar ore pulp, leave standstill 3-5min, the constant incubator being placed in 30 DEG C cultivates 48h.It is 235 that cultivation terminates rear colony number.Its solvable silicon quantity is surveyed after 5 minutes in 4000r/min centrifugal settling after this system 100 times being diluted.In solution, Dissolved Silicon increases by 30.4%.Show that silicate bacteria is well-adjusted in v-ti magnetite ore pulp.
Embodiment 3: the biological desiliconization of agar ore pulp
5% agar ore pulp: sucrose 1.04g, NaH
2pO
40.40g, MgSO
47H
2o0.12g, FeCl
30.0013g, CaCO
30.0239g, vanadium titano-magnetite 10.25g, agar 3.03g, distilled water 200mL, pH7.5.Silicate bacteria after cultivating is inoculated in slant medium, in 30 DEG C of constant incubators, cultivates 24h, pour in the beaker containing 300ml sterile purified water, make bacteria suspension 1; With the pipette, extract 1ml bacteria suspension 1 of sterilizing in containing in the beaker of 100ml sterile purified water, make bacteria suspension 2; With the pipette, extract 2ml bacteria suspension 2 of sterilizing in containing in the beaker of 100ml sterile purified water, make bacteria suspension 3.Draw 1ml bacteria suspension 3 in 5% agar ore pulp, leave standstill 3-5min, the constant incubator being placed in 30 DEG C cultivates 48h.It is 12 that cultivation terminates rear colony number.The bacterial body density of bacteria suspension 3 is minimum, and this value still can illustrate that silicate bacteria has good adaptability in v-ti magnetite ore pulp.Its solvable silicon quantity is surveyed after 5 minutes in 4000r/min centrifugal settling after this system 100 times being diluted.In solution, Dissolved Silicon increases by 18.7%.
Embodiment 4: the biological desiliconization of biological leaching silicon ore pulp
2% biological leaching silicon ore pulp: sucrose 5.00g, NaH
2pO
42.02g, MgSO
47H
2o0.50g, FeCl
30.0055g, CaCO
30.11g, vanadium titano-magnetite (crossing 180 mesh sieves) 20.16g, distilled water 1000mL, pH7.5.Silicate bacteria after inoculation culture is in containing in 2% bioleaching ore pulp.Substratum after above-mentioned process is put into constant temperature oscillator, 30 DEG C, 110rpm, cultivate 7 days.With this understanding, in solution, Dissolved Silicon concentration adds 24.6%.Bacterium to the immersion Zn of silicon in vanadium titano-magnetite clearly.
Embodiment 5: the biological desiliconization of biological leaching silicon ore pulp
2% biological leaching silicon ore pulp: starch 5.00g, NaH
2pO
42.00g, MgSO
47H
2o0.51g, FeCl
30.0052g, CaCO
30.11g, vanadium titano-magnetite (crossing 40 mesh sieves) 20.12g, distilled water 1000mL, pH7.5.Silicate bacteria after inoculation culture is in containing in 2% bioleaching ore pulp.Substratum after above-mentioned process is put into constant temperature oscillator, 30 DEG C, 110rpm, cultivate 7 days.With this understanding, in solution, Dissolved Silicon concentration adds 10.3%.Although the granularity of vanadium titano-magnetite is comparatively large, bacterium is comparatively obvious to the immersion Zn of silicon in vanadium titano-magnetite.
Embodiment 6: the biological desiliconization of silicate bacteria pre-fermentation broth
Silicate bacteria pre-fermentation broth: starch 6.00g, NaH
2pO
42.02g, MgSO
47H
2o0.51g, FeCl
30.0056g, CaCO
30.10g, vanadium titano-magnetite 0g, distilled water 1000mL, pH7.5.Bacterial classification after inoculation culture, in silicate bacteria pre-fermentation broth, puts into constant temperature oscillator, 30 DEG C, 110rpm, cultivates 7 days.After fermentation ends, get 100mL bacteria suspension and add 1g vanadium titano-magnetite (crossing 40 mesh sieves), be placed on 30 DEG C, cultivate 4 days in the constant temperature oscillator of 110rpm.With this understanding, in solution, Dissolved Silicon relative concentration adds 13.9% in deactivation comparative sample.Although the granularity of vanadium titano-magnetite is comparatively large, bacterium is still obvious to the immersion Zn of silicon in vanadium titano-magnetite.
Claims (5)
1. the Biological desiliconization method of vanadium titano-magnetite, is characterized in that: comprise the steps:
A, cultivation silicate bacteria:
1) get silicate bacteria, described silicate bacteria is colloid bacillus powder;
2) substratum is prepared: the component containing following weight proportioning:
Every 1000ml distilled water adds 4-6g glucide, 0.25-0.78g in the water-soluble phosphorus containg substances of P, 30-70mg in the magnesium salts of Mg, 1-2.8mg in the molysite of Fe, 32-65mg in the calcium salt of Ca, 0.5-10g vanadium titano-magnetite, 10-20g jelling agent; Control ph 7-8;
3) silicate bacteria add water make concentration be 0.1% ~ 0.0001% bacteria suspension be placed in step 2) gained substratum cultivates, and obtains the silicate bacteria after cultivating;
Wherein, bacteria suspension is added in following ratio: substratum 50g adds 0.1-2ml bacteria suspension and cultivates;
B, pulverizing vanadium titano-magnetite are to crossing 40-400 mesh sieve;
C, biological desiliconization:
1) preparation biological leaching silicon ore pulp: the component containing following weight proportioning:
Add 3-5.2g glucide in every 1000mL water, 0.43-1.03g in the water-soluble phosphorus containg substances of P, 1-50mg in the magnesium salts of Mg, 0.34-3.44mg in the molysite of Fe, 4-60mg in the calcium salt of Ca, 8-100g vanadium titano-magnetite; Control ph 7-8;
2) desiliconization is cultivated: the silicate bacteria after steps A cultivation adds in biological leaching silicon ore pulp, and temperature controls at 20-40 DEG C, and cultivate 5-15 days, vanadium titano-magnetite separates out Dissolved Silicon to solution, and solid-liquid separation gets final product desiliconization;
Or
1) prepare silicate bacteria pre-fermentation broth, the silicate bacteria after inoculation step A cultivates, temperature controls at 25-35 DEG C, cultivates 7-14 days, obtains fermented liquid;
Pre-fermentation broth contains the component of following weight proportioning:
Every 1000ml distilled water adds 4-6g glucide, and 0.52-1.29g is in the water-soluble phosphorus containg substances of P, and 9.8-69mg is in the magnesium salts of Mg, and 1-2.8mg is in the molysite of Fe, and 12-64mg is in the calcium salt of Ca; Control ph 7-8;
2) to step 1) add vanadium titano-magnetite in gained fermented liquid, control pulp density 2%-12%, temperature controls at 10-40 DEG C, and cultivate 2-10 days, vanadium titano-magnetite separates out Dissolved Silicon to solution, and solid-liquid separation gets final product desiliconization.
2. the Biological desiliconization method of vanadium titano-magnetite according to claim 1, is characterized in that: steps A jelling agent is agar, gelatin, silica gel, water soluble polyacrylic or water soluble cellulose class.
3. the Biological desiliconization method of vanadium titano-magnetite according to claim 1, is characterized in that: glucide described in step C is sucrose, glucose, fructose or starch.
4. the Biological desiliconization method of vanadium titano-magnetite according to claim 1, is characterized in that: nonnitrogenous in water-soluble phosphorus containg substances described in step C, potassium, magnesium, calcium or iron.
5. the Biological desiliconization method of vanadium titano-magnetite according to claim 1, is characterized in that: water-soluble phosphorus containg substances described in step C is NaH
2pO
4, Na
2hPO
4or acid phosphate zinc.
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| CN102168171A (en) * | 2011-03-10 | 2011-08-31 | 河南省岩石矿物测试中心 | Novel biological desilication purification process for rutile rough concentrate |
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| CN102168171A (en) * | 2011-03-10 | 2011-08-31 | 河南省岩石矿物测试中心 | Novel biological desilication purification process for rutile rough concentrate |
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