CN113912072A - High-efficiency purification method of low-grade clay mineral - Google Patents
High-efficiency purification method of low-grade clay mineral Download PDFInfo
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- CN113912072A CN113912072A CN202111176355.2A CN202111176355A CN113912072A CN 113912072 A CN113912072 A CN 113912072A CN 202111176355 A CN202111176355 A CN 202111176355A CN 113912072 A CN113912072 A CN 113912072A
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- 238000000034 method Methods 0.000 title claims abstract description 47
- 239000002734 clay mineral Substances 0.000 title claims abstract description 31
- 238000000746 purification Methods 0.000 title claims abstract description 17
- RYYXDZDBXNUPOG-UHFFFAOYSA-N 4,5,6,7-tetrahydro-1,3-benzothiazole-2,6-diamine;dihydrochloride Chemical compound Cl.Cl.C1C(N)CCC2=C1SC(N)=N2 RYYXDZDBXNUPOG-UHFFFAOYSA-N 0.000 claims abstract description 20
- 230000005291 magnetic effect Effects 0.000 claims abstract description 15
- 239000012141 concentrate Substances 0.000 claims abstract description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 53
- 229910052742 iron Inorganic materials 0.000 claims description 23
- 239000006148 magnetic separator Substances 0.000 claims description 23
- 239000002245 particle Substances 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 15
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 14
- 239000010936 titanium Substances 0.000 claims description 14
- 229910052719 titanium Inorganic materials 0.000 claims description 14
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 12
- 238000004062 sedimentation Methods 0.000 claims description 12
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 7
- 239000004576 sand Substances 0.000 claims description 7
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical group [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 6
- 239000002270 dispersing agent Substances 0.000 claims description 6
- 239000008394 flocculating agent Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 6
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 6
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 3
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 229910001447 ferric ion Inorganic materials 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 235000019353 potassium silicate Nutrition 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 238000004537 pulping Methods 0.000 claims description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 3
- 239000011707 mineral Substances 0.000 abstract description 26
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 25
- 238000007885 magnetic separation Methods 0.000 abstract description 13
- 230000009467 reduction Effects 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 9
- 239000012535 impurity Substances 0.000 abstract description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 8
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- KEHCHOCBAJSEKS-UHFFFAOYSA-N iron(2+);oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[O-2].[Ti+4].[Fe+2] KEHCHOCBAJSEKS-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 239000004408 titanium dioxide Substances 0.000 abstract description 2
- 229910052625 palygorskite Inorganic materials 0.000 description 9
- JVBXVOWTABLYPX-UHFFFAOYSA-L sodium dithionite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 229960000892 attapulgite Drugs 0.000 description 7
- 239000004927 clay Substances 0.000 description 6
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 3
- 229910052595 hematite Inorganic materials 0.000 description 3
- 239000011019 hematite Substances 0.000 description 3
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000005995 Aluminium silicate Substances 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 239000004113 Sepiolite Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 235000012211 aluminium silicate Nutrition 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000000440 bentonite Substances 0.000 description 2
- 229910000278 bentonite Inorganic materials 0.000 description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 229910052626 biotite Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- -1 papermaking Substances 0.000 description 2
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 2
- 229910052683 pyrite Inorganic materials 0.000 description 2
- 239000011028 pyrite Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 229910052624 sepiolite Inorganic materials 0.000 description 2
- 235000019355 sepiolite Nutrition 0.000 description 2
- 229910021646 siderite Inorganic materials 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 210000002268 wool Anatomy 0.000 description 2
- 229910021532 Calcite Inorganic materials 0.000 description 1
- PMVSDNDAUGGCCE-TYYBGVCCSA-L Ferrous fumarate Chemical compound [Fe+2].[O-]C(=O)\C=C\C([O-])=O PMVSDNDAUGGCCE-TYYBGVCCSA-L 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- RRHLZIGGSSXCMX-UHFFFAOYSA-L [Fe+2].S(=O)([O-])S(=O)[O-].[Na+] Chemical compound [Fe+2].S(=O)([O-])S(=O)[O-].[Na+] RRHLZIGGSSXCMX-UHFFFAOYSA-L 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
- 235000019728 animal nutrition Nutrition 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229910001919 chlorite Inorganic materials 0.000 description 1
- 229910052619 chlorite group Inorganic materials 0.000 description 1
- QBWCMBCROVPCKQ-UHFFFAOYSA-N chlorous acid Chemical compound OCl=O QBWCMBCROVPCKQ-UHFFFAOYSA-N 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000010459 dolomite Substances 0.000 description 1
- 229910000514 dolomite Inorganic materials 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 230000003031 feeding effect Effects 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 229910001608 iron mineral Inorganic materials 0.000 description 1
- IXQWNVPHFNLUGD-UHFFFAOYSA-N iron titanium Chemical compound [Ti].[Fe] IXQWNVPHFNLUGD-UHFFFAOYSA-N 0.000 description 1
- 230000005381 magnetic domain Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000011022 opal Substances 0.000 description 1
- 230000005298 paramagnetic effect Effects 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229910052952 pyrrhotite Inorganic materials 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052604 silicate mineral Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- BUUPQKDIAURBJP-UHFFFAOYSA-N sulfinic acid Chemical compound OS=O BUUPQKDIAURBJP-UHFFFAOYSA-N 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 229910052613 tourmaline Inorganic materials 0.000 description 1
- 239000011032 tourmaline Substances 0.000 description 1
- 229940070527 tourmaline Drugs 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/40—Clays
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
- B03B7/00—Combinations of wet processes or apparatus with other processes or apparatus, e.g. for dressing ores or garbage
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
- B03B9/00—General arrangement of separating plant, e.g. flow sheets
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
A high-efficiency purification method of low-grade clay minerals adopts a novel process of removing magnetic minerals by superconducting magnetic separation and then removing iron (titanium) oxide in clay mineral concentrates by a thiourea dioxide reduction method. The method is characterized in that a physical (superconducting magnetic separation) method and a chemical (reduction) method are combined, so that the effect of efficiently removing metal impurities is achieved, the method is superior to the traditional method, the impurity removal effect is 1+1>2, and the purified mineral with the content of iron oxide less than 0.15% and the content of titanium dioxide less than 0.02% is obtained.
Description
Technical Field
The invention belongs to the field of clay mineral purification, and particularly relates to a high-efficiency purification method of a low-grade clay mineral.
Background
Clay minerals are the main minerals that make up claystone and soil. They are a group of hydrous silicate minerals mainly containing aluminum, magnesium and the like. The clay minerals include kaolin, bentonite, attapulgite, sepiolite, palygorskite and other minerals, except the sepiolite and the palygorskite which have chain layered structures, most of the clay minerals have layered structures, the particles are extremely fine, the size is generally smaller than the micron grade, and the clay minerals have plasticity of different degrees after being added with water.
The clay mineral has wide application in various industries of national economy. Wherein, the kaolin is mainly used for ceramic raw materials, papermaking, rubber fillers, coatings, refractory materials and oil refining catalysts; the bentonite is mainly used as a catalyst and a bleaching agent for drilling mud and refining petroleum, a binder for iron ore pellets and a foundry sand binder; attapulgite clay (attapulgite), clay mainly comprising water-containing magnesium-rich silicate (attapulgite) with a layer-chain transition structure, has very high use value because of its excellent thickening property, suspension property and suspension property, and is widely applied to the paint and paint industries in developed countries, but the attapulgite clay usually coexists with minerals such as dolomite, calcite, quartz, opal and the like, so that the purity of the attapulgite clay is not high, and the use effect and the use range are directly influenced. In addition, the attapulgite clay is also reported in the research of animal nutrition, and can be used as a feed additive to replace antibiotics to promote the growth of animals so as to obtain a better feeding effect.
However, the non-metal ore is mined for many years without restriction, so that the reserves of domestic high-quality clay resources are sharply reduced in recent years, the quality of the resources is sharply reduced, the ore content of raw ore is only 15% -22%, and the content of impurity minerals such as silicon dioxide, feldspar, mica and the like is more than 70%. In addition, the iron and titanium content of the mineral obtained by the existing mineral separation and purification method is high, and the requirement of the high-grade application field is difficult to meet, so that a more effective purification method for low-grade clay mineral is developed urgently.
Disclosure of Invention
The invention provides a high-efficiency purification method of a low-grade clay mineral, and aims to solve the problem that the removal of iron and titanium by the traditional clay mineral purification method cannot meet the requirements of high-grade application fields.
In order to achieve the purpose, the invention adopts the technical scheme that:
a high-efficiency purification method of low-grade clay minerals is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps of firstly, crushing raw clay mineral ores, sequentially adding water and a dispersant for pulping to obtain coarse ore pulp with the solid content of 10% -30%, wherein the dispersant is a mixture of sodium hydroxide and sodium hexametaphosphate, and the weight ratio of the sodium hydroxide to the sodium hexametaphosphate is 1: 10-1: 15;
secondly, the coarse ore pulp is screened by a vibrating screen with 50-70 meshes to remove coarse sand, and then a phi 250mm swirler is used to remove fine sand on the upper layer, so as to obtain primary purified ore pulp;
thirdly, adding water glass into the primary purified ore pulp to adjust the pH value to 7-9, adding sodium polyacrylate, wherein the addition amount of the sodium polyacrylate is 0.1-0.5% of the mass of the raw ore dry ore of the clay mineral, and fully stirring and uniformly mixing until the sodium polyacrylate is completely dissociated and dispersed in the ore pulp;
and fourthly, conveying the ore pulp uniformly mixed with the sodium polyacrylate in the third step to a sedimentation tank for sedimentation, measuring the temperature of the ore pulp in the sedimentation tank and the liquid level height of the ore pulp, and calculating the sedimentation time according to a Stokes law simplified empirical formula, wherein the Stokes law simplified empirical formula is as follows: t ═ Tn×h/d2Wherein T represents the settling time, n represents the temperature in centigrade, h represents the pulp liquid level height in centimeters, d represents the expected settled particle size in micrometers, the calculation takes 7, TnExpressing the temperature coefficient, and looking up the table to obtain T according to the temperature comparison table of the formula corresponding to the measured temperature valuenValues, the temperature look-up table is:
standing for the settling time, wherein the particle size of the particles of the lower-layer ore pulp in the settling pond is more than 7 microns, and the particle size of the particles of the upper-layer ore pulp is less than 7 microns after the settling is finished;
fifthly, adjusting the solid content of the upper layer ore pulp with the particle size of less than 7 microns to 15% -25%, feeding the upper layer ore pulp into a superconducting magnetic separator, setting the magnetic field of the superconducting magnetic separator to be 5T, and setting the flow speed of the ore pulp to be 21-35 m3H, removing iron and titanium;
sixthly, adjusting the solid content concentration of the ore pulp subjected to iron and titanium removal by the superconducting magnetic separator to be 18-22%, adding thiourea dioxide to reduce the residual iron element in the ore pulp to be in a positive trivalent state, wherein the addition amount of the thiourea dioxide is 3-5 per mill of the solid content of the ore pulp subjected to iron and titanium removal by the superconducting magnetic separator, fully stirring uniformly, standing for 1 hour, adding citric acid to convert the iron element in the ore pulp into ionic positive ferric ions, and the addition amount of the citric acid is 1-1.5 per mill of the solid content of the ore pulp subjected to iron and titanium removal by the superconducting magnetic separator, fully stirring, and reacting for 1 hour;
and step seven, adding a flocculating agent into the ore pulp after the reaction in the step six, fully and uniformly stirring, and performing filter pressing and dehydration to obtain the clay mineral concentrate.
In the first step, raw clay mineral ores are crushed to be less than 3-5 mm.
In the fifth step, the flow rate of the mixture fed into the superconducting magnetic separator is 25-31 m3/h。
The flocculating agent is aluminum sulfate, and the addition amount of the aluminum sulfate is 1-3 per mill of the dry ore content of the ore pulp subjected to iron removal by the superconducting magnetic separator.
The design principle and the effect of the invention are as follows:
1. the technical scheme of the invention combines impurity removal and thiourea dioxide reduction by using a superconducting magnetic separator:
the method for removing iron (titanium) by superconducting magnetic separation has obvious effect on removing weakly magnetic minerals which are difficult to separate by the traditional electromagnetic separation (magnetic field is 1.3T-1.6T), especially limonite, magnetite, hematite, pyrite, siderite and the like.
The weakly magnetic minerals mostly belong to paramagnetic substances, do not have magnetic domain structures, are much weaker in magnetism than the strongly magnetic minerals, are irrelevant to factors such as the shape and the granularity of the minerals, are determined only by the composition and the structure of the minerals, and roughly comprise: biotite, limonite, pyrite, hematite, chlorite, tourmaline, rutile, and the like. The minerals are difficult to remove by a simple electromagnetic separation method, and can only be removed by a superconducting magnetic separation method.
The processing step of the superconducting magnetic separation can remove a plurality of types of magnetic iron-containing minerals (including strong magnetic minerals such as magnetite, ilmenite, pyrrhotite, ferrozinc spinel and the like, weak magnetic minerals such as hematite, limonite, siderite, ilmenite, biotite, manganite and the like), but certain defects exist, the superconducting magnetic separation rapidly flows into a cavity of a superconducting machine through ore pulp, the magnetic minerals are mostly adsorbed when passing through steel wool in the cavity, however, in consideration of the capacity machine and the economy of equipment, the ore pulp needs to pass through the cavity at a certain flow rate, the contact rate of the ore pulp and the steel wool is limited to a certain extent, not 100 percent of the magnetic mineral can be contacted, and a small part of the magnetic mineral is not adsorbed;
secondly, the reducing agent adopting a chemical method can permeate into mineral molecules, and due to a chemical reaction, the iron oxide can be basically removed as long as the ore pulp is uniformly stirred and the reaction time is enough, but only one iron mineral can be removed, and the iron removal range is narrow;
the two are combined, firstly, superconducting magnetic separation is used for removing impurities, and then thiourea dioxide is used for reducing and removing iron, so that the impurity removing effect can reach 1+1 to 2, and the purified mineral with the iron oxide content of less than 0.15% and the titanium dioxide content of less than 0.02% is obtained.
2. Selection of thiourea dioxide:
the sodium hydrosulfite iron removal method is a traditional iron removal method, and the process method is simple, feasible and easy to operate, but the method has the defects that the reaction condition is under an acidic condition, and the environment is not friendly; and the sodium hydrosulfite is decomposed fast usually under natural conditions, the decomposition of the sodium hydrosulfite is accelerated along with the reaction, the utilization rate of the sodium hydrosulfite is greatly reduced, and the iron removal effect is poor and the environment is polluted.
Therefore, the technical scheme adopts a thiourea dioxide reduction deferrization method to further deferrize the settled ore pulp, the reaction condition of the method is alkalescence, the ore pulp subjected to superconducting magnetic separation is alkalescence, and the pH value of the ore pulp does not need to be adjusted by adding sulfuric acid (which is also an important advantage of the technical scheme), namely the ore pulp subjected to superconducting magnetic separation directly enters a reaction tank for reaction.
This technical scheme uses thiourea dioxide to replace traditional sodium hydrosulfite, compares with sodium hydrosulfite and has advantages such as the reducibility is strong, the thermostability is good, the storage transportation is convenient, and the concrete performance is:
firstly, sulfinic acid with strong reducibility is generated by decomposition under an alkaline condition, and the reducibility is controllable;
thiourea dioxide has higher reduction potential, and the reduction potential is slowly reduced by only 20 percent of the reduction potential of the sodium hydrosulfite;
the thiourea dioxide has good safety performance and no pollution during production and use;
thiourea dioxide is a stable compound and is not dangerous. The sodium hydrosulfite often has explosion phenomenon in the field use process.
Thiourea dioxide contains little sulfide odor, and is safe in operation environment and sanitation.
The method is a new process for removing magnetic minerals by superconducting magnetic separation and then removing iron (titanium) oxide in clay mineral concentrate by a thiourea dioxide reduction method. The method is characterized in that a physical (superconducting magnetic separation) method and a chemical (reduction) method are combined, so that the effect of efficiently removing the metal impurities is achieved, and the method is superior to the traditional method.
Detailed Description
Example (b): high-efficiency purification method of low-grade clay mineral
A high-efficiency purification method of low-grade clay minerals is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps of firstly, crushing raw clay mineral ores to the size of less than 3-5mm, sequentially adding water and a dispersing agent for pulping to obtain coarse ore pulp with the solid content of 10% -30%, wherein the dispersing agent is a mixture of sodium hydroxide and sodium hexametaphosphate, and the weight ratio range of the sodium hydroxide to the sodium hexametaphosphate is 1: 10-1: 15;
secondly, the coarse ore pulp is screened by a vibrating screen with 50-70 meshes to remove coarse sand, and then a phi 250mm swirler is used to remove fine sand on the upper layer, so as to obtain primary purified ore pulp;
thirdly, adding water glass into the primary purified ore pulp to adjust the pH value to 7-9, adding sodium polyacrylate, wherein the addition amount of the sodium polyacrylate is 0.1-0.5% of the mass of the raw ore dry ore of the clay mineral, and fully stirring and uniformly mixing until the sodium polyacrylate is completely dissociated and dispersed in the ore pulp;
and fourthly, conveying the ore pulp uniformly mixed with the sodium polyacrylate in the third step to a sedimentation tank for sedimentation, measuring the temperature of the ore pulp in the sedimentation tank and the liquid level height of the ore pulp, and calculating the sedimentation time according to a Stokes law simplified empirical formula, wherein the Stokes law simplified empirical formula is as follows: t ═ Tn×h/d2Wherein T represents the settling time, n represents the temperature in centigrade, h represents the pulp liquid level height in centimeters, d represents the expected settled particle size in micrometers, the calculation takes 7, TnExpressing the temperature coefficient, and looking up the table to obtain T according to the temperature comparison table of the formula corresponding to the measured temperature valuenValues, the temperature look-up table is:
standing for the settling time, wherein the particle size of the particles of the lower-layer ore pulp in the settling pond is more than 7 microns, and the particle size of the particles of the upper-layer ore pulp is less than 7 microns after the settling is finished;
fifthly, adjusting the solid content of the upper layer ore pulp with the particle size of less than 7 microns to 15% -25%, feeding the upper layer ore pulp into a superconducting magnetic separator, setting the magnetic field of the superconducting magnetic separator to be 5T, and setting the flow speed of the ore pulp to be 21-35 m3H, removing iron and titanium;
sixthly, adjusting the solid content concentration of the ore pulp subjected to iron and titanium removal by the superconducting magnetic separator to be 18-22%, adding thiourea dioxide to reduce the residual iron element in the ore pulp to be in a positive trivalent state, wherein the addition amount of the thiourea dioxide is 3-5 per mill of the solid content of the ore pulp subjected to iron and titanium removal by the superconducting magnetic separator, fully stirring uniformly, standing for 1 hour, adding citric acid to convert the iron element in the ore pulp into ionic positive ferric ions, and the addition amount of the citric acid is 1-1.5 per mill of the solid content of the ore pulp subjected to iron and titanium removal by the superconducting magnetic separator, fully stirring, and reacting for 1 hour;
and seventhly, adding a flocculating agent into the ore pulp after the reaction in the sixth step, fully and uniformly stirring, and performing filter pressing and dehydration to obtain clay mineral concentrate, wherein the flocculating agent is aluminum sulfate, and the addition amount of the aluminum sulfate is 1-3 per mill of the dry ore amount of the ore pulp subjected to iron removal by the superconducting magnetic separator.
In the fifth step, the flow rate of the mixture fed into the superconducting magnetic separator is 25-31 m3/h。
Table 1 below shows the impurity data of the clay mineral concentrate obtained in example 1:
table 1:
| item | Fe2O3(％) | TiO2(％) | Whiteness degree |
| Coarse mineral dressing | 0.58 | 0.28 | 78 |
| Superconducting ore | 0.29 | 0.02 | 88 |
| Ore after reduction of thiourea dioxide | 0.15 | 0.02 | 92 |
The information of the superconducting magnetic separator in the embodiment is as follows:
TABLE 2 superconducting magnet separator information
TABLE 3 purification results of superconducting magnetic separation and impurity removal under different flow rates
As can be seen from Table 3, the purifying effect of the superconducting magnetic separation becomes better gradually along with the reduction of the flow rate of the ore pulp, namely the Fe in the minerals2O3And TiO2The content gradually decreases as the pulp flow rate decreases.But a moderate flow rate needs to be selected in view of economic efficiency.
Comparative example 1:
TABLE 4 comparison of crude beneficiation with ore indexes after sodium hydrosulfite/thiourea dioxide reduction
| Item | Fe2O3(％) | Ti O2(％) | Whiteness degree |
| Coarse mineral dressing | 0.58 | 0.28 | 78 |
| After the sodium hydrosulfite is reduced | 0.51 | 0.28 | 80 |
| After thiourea dioxide reduction | 0.41 | 0.28 | 82 |
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (4)
1. A high-efficiency purification method of low-grade clay minerals is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps of firstly, crushing raw clay mineral ores, sequentially adding water and a dispersant for pulping to obtain coarse ore pulp with the solid content of 10% -30%, wherein the dispersant is a mixture of sodium hydroxide and sodium hexametaphosphate, and the weight ratio of the sodium hydroxide to the sodium hexametaphosphate is 1: 10-1: 15;
secondly, the coarse ore pulp is screened by a vibrating screen with 50-70 meshes to remove coarse sand, and then a phi 250mm swirler is used to remove fine sand on the upper layer, so as to obtain primary purified ore pulp;
thirdly, adding water glass into the primary purified ore pulp to adjust the pH value to 7-9, adding sodium polyacrylate, wherein the addition amount of the sodium polyacrylate is 0.1-0.5% of the mass of the raw ore dry ore of the clay mineral, and fully stirring and uniformly mixing until the sodium polyacrylate is completely dissociated and dispersed in the ore pulp;
and fourthly, conveying the ore pulp uniformly mixed with the sodium polyacrylate in the third step to a sedimentation tank for sedimentation, measuring the temperature of the ore pulp in the sedimentation tank and the liquid level height of the ore pulp, and calculating the sedimentation time according to a Stokes law simplified empirical formula, wherein the Stokes law simplified empirical formula is as follows: t ═ Tn×h/d2Wherein T represents the settling time, n represents the temperature in centigrade, h represents the pulp liquid level height in centimeters, d represents the expected settled particle size in micrometers, the calculation takes 7, TnExpressing the temperature coefficient, and looking up the table to obtain T according to the temperature comparison table of the formula corresponding to the measured temperature valuenValues, the temperature look-up table is:
standing for the settling time, wherein the particle size of the particles of the lower-layer ore pulp in the settling pond is more than 7 microns, and the particle size of the particles of the upper-layer ore pulp is less than 7 microns after the settling is finished;
fifthly, adjusting the solid content of the upper layer ore pulp with the particle size of less than 7 microns to 15% -25%, feeding the upper layer ore pulp into a superconducting magnetic separator, setting the magnetic field of the superconducting magnetic separator to be 5T, and setting the flow speed of the ore pulp to be 21-35 m3H, removing iron and titanium;
sixthly, adjusting the solid content concentration of the ore pulp subjected to iron and titanium removal by the superconducting magnetic separator to be 18-22%, adding thiourea dioxide to reduce the residual iron element in the ore pulp to be in a positive trivalent state, wherein the addition amount of the thiourea dioxide is 3-5 per mill of the solid content of the ore pulp subjected to iron and titanium removal by the superconducting magnetic separator, fully stirring uniformly, standing for 1 hour, adding citric acid to convert the iron element in the ore pulp into ionic positive ferric ions, and the addition amount of the citric acid is 1-1.5 per mill of the solid content of the ore pulp subjected to iron and titanium removal by the superconducting magnetic separator, fully stirring, and reacting for 1 hour;
and step seven, adding a flocculating agent into the ore pulp after the reaction in the step six, fully and uniformly stirring, and performing filter pressing and dehydration to obtain the clay mineral concentrate.
2. The efficient purification method according to claim 1, wherein: in the first step, raw clay mineral ores are crushed to be less than 3-5 mm.
3. The efficient purification method according to claim 1, wherein: in the fifth step, the flow rate of the mixture fed into the superconducting magnetic separator is 25-31 m3/h。
4. The efficient purification method according to claim 1, wherein: the flocculating agent is aluminum sulfate, and the addition amount of the aluminum sulfate is 1-3 per mill of the dry ore content of the ore pulp subjected to iron removal by the superconducting magnetic separator.
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