CN100457619C - Method of preparing calcium silicate powder from multi-metal tailings - Google Patents
Method of preparing calcium silicate powder from multi-metal tailings Download PDFInfo
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- CN100457619C CN100457619C CNB2007100987441A CN200710098744A CN100457619C CN 100457619 C CN100457619 C CN 100457619C CN B2007100987441 A CNB2007100987441 A CN B2007100987441A CN 200710098744 A CN200710098744 A CN 200710098744A CN 100457619 C CN100457619 C CN 100457619C
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Abstract
This invention relates to a method for preparing CaSiO3 powder from multi-metal PbZn gangues including: crushing, calcining, filtering, depositing for four times, dissolving, depositing and calcining, which is advantaged that it can recover many kinds of valuable metal elements the same time when preparing CaSiO3 from the gangues containing low grade of Ca, and the purity of the product is high and can be used in plastics, polymer, dope, dye, ceramics, metallurgy, building materials, environmental protection and substitutes of asbestos.
Description
Technical field
The invention belongs to the colored metallurgical industrial technical field, proposed a kind of method that from many metals Pb-Zn tailings, prepares calcium silicate powder, have advantages of high practicability.
Background technology
Along with China's mine resources is constantly exploited, the mine waste also constantly increases, and this has not only caused the waste of resource, also environment has been brought great pressure.Statistic data shows that the annual mine tailing that produces of China bargh has 26.15 hundred million t approximately, and the comprehensive reutilization amount is 11.8 hundred million t, and the comprehensive reutilization rate is 6.95%, and mine tailing storehouse floor space adds up to 37282hm
2, and increasing with annual 500000000 tons speed.Therefore, seek that rational approach is disposed mine tailing and utilization seems particularly urgent.
Calcium silicate powder has that capacity is little, thermal conductivity is little, adsorptivity is big, resistance to compression, folding strength are big, therefore advantages such as temperature height, easy construction, the wastage rate of being born during use are low, can repeat to utilize again are widely used in the piping insulation in the industries such as oil, light industry, metallurgy, electric power, building materials; Owing to its unique physical and chemical performance and mineralogical characteristic, also be applied in addition at the aspects such as surrogate of plastics, rubber, polymkeric substance, coating, dyestuff, pottery, metallurgy, building materials, environmental protection and asbestos.
The wet chemical method of the preparation calcium silicate powder that present China is used mainly contains the precipitator method, spray pyrolysis, sol-gel method, hydrothermal method, micro emulsion method, gamma-radiation method etc., the used calcareous starting material of these methods mainly are lime or asbestos, their purity is all than higher, and the dispersion effect in solution is better.The method for preparing calcium silicate powder that the present invention is used, raw material low to grade, the dispersing property difference has important meaning.
Summary of the invention
The object of the present invention is to provide a kind of method that from multi-metal tailings, prepares calcium silicate powder, the one, mine tailing is carried out the recovery of valuable element, realized the comprehensive utilization of resource; The 2nd, prepared calcium silicate powder can be directly used in the preparation of other materials such as lagging material and pottery, has reduced cost.
Processing step of the present invention is as follows:
(1) pulverize: raw material is carried out ore grinding, cross the 0.074mm sieve, described raw material is a mine tailing.
(2) calcining: the mineral after will pulverizing carry out sulphur removal 750-900 ℃ of calcining 3～4 hours.
(3) filter: double-deck filter paper filtering, remove SiO
2
(4) primary sedimentation: with NaOH solution is titrated to pH=3.0～4.0, and adds H simultaneously
2O
2, till solution colour did not change, purpose was the iron that reclaims in the solution, had also reached the purpose of cleansing soln
(5) secondary sedimentation: on the basis of primary sedimentation, control pH=7～9 of solution again, removed lead and the zinc in the solution, and can reclaim lead and zinc.
(6) three precipitations: on preceding twice sedimentary basis, control pH=12～13 of solution again, removed other outer metallic elements of stable region of oxyhydroxide.
(7) four precipitations: in the filtrate of three post precipitations, add NH
4HCO
3, till no longer including the white precipitate generation, make calcium ion with CaCO
3Form be precipitated out.
(8) dissolving: rare nitric acid is slowly dissolved above-mentioned resulting CaCO
3Precipitation, till no longer including the bubble generation, purpose is to obtain ca nitrate soln.
(9) precipitation: the polyoxyethylene glycol that adds mass percent in the above-mentioned ca nitrate soln and be 0.4-0.6% is as dispersion agent, and adding Na
2SiO
3Solution till no longer including the white precipitate generation, just obtains CaSiO
3Precipitation.
(10) calcining: with above-mentioned CaSiO
3Be deposited in 480-580 ℃ of calcining 3～4 hours, purpose is to remove crystal water, obtains CaSiO
3Powder.
The principle of the invention mainly is the difference according to metallic element ion hydrolysis pH value, because the hydrolysis pH value of calcium is bigger, by controlling different pH values, obtains the hydrolysate of other different metal elements respectively, so just realize separating of calcium and other metallic elements, in solution, added NH at last
4HCO
3, can obtain the higher CaCO of purity
3Precipitation; According to equation Na
2SiO
3+ Ca (NO
3)
2=CaSiO
3↓+2NaNO
3, with CaCO
3Be dissolved in rare nitric acid, add an amount of nitrocalcite and dispersion agent, final precipitation obtains calcium silicate powder.
Though the preparation of the wet method of present domestic calcium silicate powder is existing invention in technical field, is being that the patent of utilizing wet chemical method to prepare Calucium Silicate powder in the environmental technology field of object does not also have with mine tailing and the lower raw material of calcic grade.
The invention has the advantages that, from the lower mine tailing of calcic grade, carry out the preparation of Calucium Silicate powder, and can reclaim multiple valuable metal element simultaneously, have stronger feasibility; Prepared Calucium Silicate powder product purity is higher, can directly apply to the aspects such as surrogate of plastics, rubber, polymkeric substance, coating, dyestuff, pottery, metallurgy, building materials, environmental protection and asbestos, technological operation is simple, cost is low, environmental pollution is less, and the comprehensive utilization that realizes low grade material is had very important significance.
Description of drawings
Fig. 1 is for to prepare CaSiO from persimmon bamboo plantation Pb-Zn tailings
3Schema.
Embodiment
Below introduce the specific embodiment of the present invention by description to embodiment
Example 1:
Get the 60g raw ore and be crushed to 0.074mm, 800 ℃ of calcinings 3 hours, after the filtration, the control pH value of filtrate was 3.5, carry out sedimentation and filtration, using NaOH titration filtrate to pH=7～9, behind sedimentation and filtration, control filtrate pH=12.6 again, filter, in filtrate, add NH
4HCO
3, obtain white CaSiO
3Precipitation is with CaSiO
3Be deposited in 500 ℃ of calcinings 3 hours, final gained CaSiO
3Purity be 96.89%.
Example 2:
Get the 50g raw ore and be crushed to 0.074mm, 800 ℃ of calcinings 3 hours, after the filtration, the control pH value of filtrate was 4.0, carry out sedimentation and filtration, using NaOH titration filtrate to pH=7～9, behind sedimentation and filtration, control filtrate pH=13 again, filter, in filtrate, add NH
4HCO
3, obtain white CaSiO
3Precipitation is with CaSiO
3Be deposited in 500 ℃ of calcinings 3 hours, final gained CaSiO
3Purity be 97.26%.
Claims (1)
1, a kind of method that from many metals Pb-Zn tailings, prepares calcium silicate powder, it is characterized in that: processing step is:
A, pulverizing: raw material is carried out ore grinding, cross the 0.074mm sieve, described raw material is a mine tailing;
B, calcining: the mineral after will pulverizing carry out sulphur removal 750-900 ℃ of calcining 3～4 hours;
C, filtration: double-deck filter paper filtering, remove SiO
2
D, primary sedimentation: with NaOH solution is titrated to pH=3.0～4.0, and adds H simultaneously
2O
2, till solution colour does not change, reclaim the iron in the solution, cleansing soln;
E, secondary sedimentation: on the basis of primary sedimentation, control pH=7～9 of solution again, removed lead and the zinc in the solution, reclaim lead and zinc;
F, three precipitations: on preceding twice sedimentary basis, control pH=12～13 of solution again, removed other outer metallic elements of stable region of oxyhydroxide;
G, four precipitations: in the filtrate of three post precipitations, add NH
4HCO
3, till no longer including the white precipitate generation, make calcium ion with CaCO
3Form be precipitated out;
H, dissolving: rare nitric acid is added the above-mentioned resulting CaCO of dissolving
3Precipitation till no longer including the bubble generation, obtains ca nitrate soln;
I, precipitation: the polyoxyethylene glycol that adds mass percent in the above-mentioned ca nitrate soln and be 0.4-0.6% is as dispersion agent, and adds Na
2SiO
3Solution till no longer including the white precipitate generation, obtains CaSiO
3Precipitation;
J, calcining: with above-mentioned CaSiO
3Be deposited in 480-580 ℃ of calcining 3～4 hours, remove crystal water, obtain CaSiO
3Powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100987441A CN100457619C (en) | 2007-04-26 | 2007-04-26 | Method of preparing calcium silicate powder from multi-metal tailings |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100987441A CN100457619C (en) | 2007-04-26 | 2007-04-26 | Method of preparing calcium silicate powder from multi-metal tailings |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101033069A CN101033069A (en) | 2007-09-12 |
| CN100457619C true CN100457619C (en) | 2009-02-04 |
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ID=38729841
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2007100987441A Expired - Fee Related CN100457619C (en) | 2007-04-26 | 2007-04-26 | Method of preparing calcium silicate powder from multi-metal tailings |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102173430B (en) * | 2011-01-25 | 2012-12-12 | 昊青薪材（北京）技术有限公司 | Technique for preparing wollastonite ultrafine powder from calcium silicate hydrate |
| CN103419271A (en) * | 2012-05-23 | 2013-12-04 | 北京航空航天大学 | Preparation method of calcium silicate board |
| CN113817228A (en) * | 2021-09-28 | 2021-12-21 | 长春工业大学 | Modification method of iron-removing tailing slag |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04124227A (en) * | 1990-09-12 | 1992-04-24 | Nisshin Steel Co Ltd | Treatment of garnierite |
| CN1414121A (en) * | 2002-09-17 | 2003-04-30 | 昆明冶研新材料股份有限公司 | Method of treating low grade zinc oxide ore |
-
2007
- 2007-04-26 CN CNB2007100987441A patent/CN100457619C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04124227A (en) * | 1990-09-12 | 1992-04-24 | Nisshin Steel Co Ltd | Treatment of garnierite |
| CN1414121A (en) * | 2002-09-17 | 2003-04-30 | 昆明冶研新材料股份有限公司 | Method of treating low grade zinc oxide ore |
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| Publication number | Publication date |
|---|---|
| CN101033069A (en) | 2007-09-12 |
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Granted publication date: 20090204 Termination date: 20110426 |