CN102658242B - Mineral separation process of complex fluorite difficult to separate - Google Patents
Mineral separation process of complex fluorite difficult to separate Download PDFInfo
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- CN102658242B CN102658242B CN 201210123529 CN201210123529A CN102658242B CN 102658242 B CN102658242 B CN 102658242B CN 201210123529 CN201210123529 CN 201210123529 CN 201210123529 A CN201210123529 A CN 201210123529A CN 102658242 B CN102658242 B CN 102658242B
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- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 title claims abstract description 101
- 239000010436 fluorite Substances 0.000 title claims abstract description 97
- 229910052500 inorganic mineral Inorganic materials 0.000 title abstract description 28
- 239000011707 mineral Substances 0.000 title abstract description 28
- 238000000926 separation method Methods 0.000 title abstract description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 140
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 119
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 107
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 107
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 107
- 239000005642 Oleic acid Substances 0.000 claims abstract description 107
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 107
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 107
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 107
- 239000006260 foam Substances 0.000 claims abstract description 82
- 238000000034 method Methods 0.000 claims abstract description 58
- 239000012141 concentrate Substances 0.000 claims abstract description 46
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 39
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000004115 Sodium Silicate Substances 0.000 claims description 92
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 92
- 230000004048 modification Effects 0.000 claims description 62
- 238000012986 modification Methods 0.000 claims description 62
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 37
- 238000003756 stirring Methods 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 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 19
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 10
- -1 hydrogen sodium hydroxide Chemical class 0.000 claims description 10
- 239000000376 reactant Substances 0.000 claims description 10
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 9
- 239000000194 fatty acid Substances 0.000 claims description 9
- 229930195729 fatty acid Natural products 0.000 claims description 9
- 150000004665 fatty acids Chemical class 0.000 claims description 9
- 238000005304 joining Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 37
- 230000008569 process Effects 0.000 abstract description 18
- 239000000377 silicon dioxide Substances 0.000 abstract description 16
- 239000002253 acid Substances 0.000 abstract description 11
- 239000003795 chemical substances by application Substances 0.000 abstract description 11
- 238000005188 flotation Methods 0.000 abstract description 11
- 229910021532 Calcite Inorganic materials 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- 229910001634 calcium fluoride Inorganic materials 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 3
- 239000002351 wastewater Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 150000002889 oleic acids Chemical class 0.000 abstract description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 28
- 238000006243 chemical reaction Methods 0.000 description 18
- 229910000019 calcium carbonate Inorganic materials 0.000 description 14
- 239000007788 liquid Substances 0.000 description 12
- 238000011084 recovery Methods 0.000 description 12
- 230000004044 response Effects 0.000 description 8
- 239000002002 slurry Substances 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 7
- 238000012545 processing Methods 0.000 description 6
- 150000001669 calcium Chemical class 0.000 description 5
- 239000010453 quartz Substances 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- 239000000837 restrainer Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 230000002401 inhibitory effect Effects 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 240000004859 Gamochaeta purpurea Species 0.000 description 1
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000006011 modification reaction Methods 0.000 description 1
- 238000009856 non-ferrous metallurgy Methods 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 230000031068 symbiosis, encompassing mutualism through parasitism Effects 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a mineral separation process, in particular to a mineral separation process of complex fluorite difficult to separate. The process includes utilizing sodium hydroxide to treat oleic acid to obtain modified oleic acid, utilizing concentrated sulfuric acid to treat water glass and obtain acidized water glass, conducting ore grinding on fluorite ores according to the prior art, conducting coarse separation under the temperature of 25-30 DEG C, then conducting seven times fine separation on coarse separation foams and adding the acidized water glass into the foams in the first four times of fine separation to prepare fluorite concentrate. The process can improve separation efficiency of calcium fluoride, silica and calcite, improves quality and recycle rate of the fluorite ores, obtains high quality acid grade fluorite ores and resolves the problem of difficulty in separation of complex fluorite flotation, is remarkable in application effect in separation of the complex fluorite difficult to separate, has repeatability, simultaneously reduces requirements of fluorite mineral flotation for ore temperature, reduces energy consumption, reduces usage of collecting agent oleic acid, reduces environment pollution caused by exhaust of a large amount of waste water containing oleic acid and has better economical and social benefits.
Description
Technical field
The invention belongs to technical field of mineral processing, relate to a kind of fluorite ore ore-dressing technique, be specifically related to a kind of complicated difficult and select the fluorite ore ore-dressing technique.
Background technology
Fluorite is the primary raw material of producing fluorochemical, is widely used in again the industries such as steel-making, non-ferrous metal metallurgy, cement, glass, pottery because fusing point is low, and water white bulk fluorite crystal also can be made optics fluorite and technique fluorite.Along with advancing by leaps and bounds of world market economy, the particularly fast development of China's nonferrous metallurgy industry, grow with each passing day to the demand of acid level fluorite concentrate, thereby accelerated the progress of processing of fluorspar ores new technology.The composition of complicated fluorite ore is comparatively complicated, and fluorite mineral and quartz and calcite mineral separating difficulty are large.Traditional ore-dressing technique is heated ore pulp, uses sodium carbonate to regulate the pH value of ore pulp, with waterglass etc., suppresses gangue, with oleic acid etc. as collecting agent, through the sour grade fluorite concentrate of selected acquisitions repeatedly.Exist energy consumption high, the beneficiation reagent consumption is large, kind is many can cause environmental pollution, and, to the shortcomings such as bad adaptability of heterogeneity ore, causes complicated ingredient fluorite ore sorting index low, and concentrate quality is poor.
Summary of the invention
In order to overcome above-mentioned problems of the prior art, the purpose of this invention is to provide a kind of fluorite ore sorting index complicated difficult high, that concentrate quality is good and select the fluorite ore ore-dressing technique, alleviate the pollution to environment, strong adaptability.
For achieving the above object, the technical solution adopted in the present invention is: a kind of complicated difficult selects the fluorite ore ore-dressing technique, specifically carries out according to the following steps:
Step 1: in adding the ratio of 1 kilogram of oleic acid in 53 kg of hydrogen sodium hydroxide solution, oleic acid is added to the sodium hydroxide solution that temperature is 90 ℃~100 ℃, and stir, react fully and carry out, standing after, remove other fatty acid reactant, be cooled to room temperature, make modification oleic acid;
In adding the ratio of 3 kilograms of concentrated sulfuric acids in the double centner water glass solution, the concentrated sulfuric acid is added in water glass solution, stir, make acidified sodium silicate;
Step 2: the fluorite ore raw ore is carried out to ore grinding, obtain the ore grinding ore pulp; By ore raw ore per ton join sodium carbonate 1200 grams, density is 1.46 g/cm
3the ratio of modification oleic acid 300 grams that make of sodium silicate 1500 grams, calgon 80 grams and step 1, the modification oleic acid that the sodium carbonate of corresponding weight, waterglass, calgon and step 1 are made adds in this ore grinding ore pulp, roughly selected at the temperature of 25 ℃~30 ℃, obtained roughly selecting foam and rougher tailings;
Step 3: join the ratio of the modification oleic acid that 100 gram steps 1 make in ore raw ore per ton, this modification oleic acid of corresponding weight is added in the rougher tailings of step 2, scanned;
The ratio of joining the modification oleic acid that acidified sodium silicate that 600 gram steps 1 make and 100 gram steps 1 make in raw ore per ton, this acidified sodium silicate of corresponding weight and this modification oleic acid are added respectively to roughly selecting in foam of step 2, carry out selected for the first time, selected foam for the first time;
Step 4: join the ratio of the acidified sodium silicate that 400 gram steps 1 make in ore raw ore per ton, this acidified sodium silicate of corresponding weight added in the selected foam for the first time of step 3, carry out selected for the second time, selected foam for the second time;
Step 5: join the ratio of the acidified sodium silicate that 200 gram steps 1 make in ore raw ore per ton, this acidified sodium silicate of corresponding weight added in the selected foam for the second time of step 4, carry out selected for the third time, selected foam for the third time;
Step 6: join the ratio of the acidified sodium silicate that 100 gram steps 1 make in ore raw ore per ton, this acidified sodium silicate of corresponding weight added in the selected foam for the third time of step 5, carry out the 4th time selected, obtain selected foam the 4th time;
Step 7: by existing technique to the 4th selected foam carry out successively the 5th time selected, the 6th time selected and the 7th time selected, obtain fluorite concentrate.
NaOH and water that in described step 1, sodium hydroxide solution used is 1:340~350 by mass ratio are formulated.
In described step 1, oleic acid adds sodium hydroxide solution, stirs temperature-resistant in this Hydrogen sodium hydroxide solution 30 minutes ~ 35 minutes.
After adding thermal response and complete in described step 1, standing at least 30 minutes.
The preparation of water glass solution in described step 1: 1:3~3.5 in mass ratio are 1.46g/cm by density
3sodium silicate be added to the water, stir 15 minutes~20 minutes, make water glass solution.
In described step 1, add water glass solution to stir 25 minutes ~ 30 minutes the concentrated sulfuric acid.
Ore-dressing technique of the present invention adopts modification oleic acid soluble in water as collecting agent, reduces the requirement of fluorite to slurry temperature, has reduced collector dosage, is conducive to reduce gangue mineral and is mingled with and enters fluorite concentrate; Add calgon, acidified sodium silicate composite restrainer at flotation operation, the inhibitory action of strengthening to gangue minerals such as quartz and calcites, improve calcirm-fluoride and FLOTATION SEPARATION effect quartzy, calcite, can obtain qualified acid level fluorite concentrate, recovery rate in ore-dressing is higher, realizes the utilization of mineral resources Efficient Development.
The accompanying drawing explanation
Fig. 1 is the flow process of ore-dressing technique of the present invention.
Fig. 2 is conventional mineral processing circuit.
The specific embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Because of the gangue minerals such as quartzy calcite in complicated fluorite ore and fluorite mineral symbiosis close, disseminated grain size is superfine, and the floatability of calcite thing, quartz and fluorite mineral is close, cause the sorting difficulty, finally cause fluorite concentrate fluorinated calcium grade low, silica, calcium carbonate content are too high, affect the fluorite concentrate grade.While adopting existing flotation process processing to process complicated fluorite ore, oleic acid commonly used is as collecting agent, and the formal name used at school of this oleic acid is (Z)-9-18 (carbon) olefin(e) acid, is a kind of aliphatic acid, molecular formula C
18h
34o
2, molecular weight 282.47, skeleton symbol CH
3(CH
2)
7cH=CH (CH
2)
7cOOH; Be soluble in the organic solvents such as ethanol, ether, chloroform, water insoluble.While adopting oleic acid as the fluorite mineral collector, in the situation that temperature is lower, its consumption is often larger, particularly in the northern area of China, winter temperature is through being everlasting below zero degrees celsius, and the oleic acid consumption often exceeds than the summer more than one times, and the use of a large amount of oleic acid not only can increase beneficiation cost, worsens floatation process, affect sorting index, and in beneficiation wastewater, the existence of a large amount of oleic acid has increased the pollution to environment, is badly in need of taking measures to solve.The technological means adopted during most of fluorite ore ore dressing is the heating ore pulp, slurry temperature is brought up to 35~40 ℃, add again oleic acid, to increase the solubility of oleic acid in ore pulp, improve its dispersion effect in ore pulp, reach the purpose that reduces the oleic acid consumption, but the heating ore pulp can make floatation process complicated, consume a large amount of energy, increase beneficiation cost.Therefore, the use of this technique is subject to many limitations.
In order to overcome above-mentioned problems of the prior art, the invention provides the ore-dressing technique that a kind of complicated difficult selects fluorite ore, adopt collecting agent soluble in water, reduce the requirement of flotation to slurry temperature, reduced the consumption of collecting agent, the minimizing gangue mineral is mingled with clamp-ons fluorite concentrate, improves sorting index, obtain qualified acid level fluorite concentrate, improved beneficiating efficiency.This ore-dressing technique is specifically carried out according to the following steps:
Step 1: 1:340~350 in mass ratio, get respectively NaOH and water, be made into sodium hydroxide solution, steam is passed into to this sodium hydroxide solution, make the temperature of sodium hydroxide solution rise to 90~100 ℃, in adding the ratio of 1 kilogram of oleic acid in 53 kg of hydrogen sodium hydroxide solution, oleic acid is added in the sodium hydroxide solution after intensification, stir 30~35 minutes, react fully and carry out, continue to pass into steam in the process that adds oleic acid and stir in sodium hydroxide solution, make reaction temperature remain at 90~100 ℃, after adding thermal response and completing, stop passing into steam, standing at least 30 minutes, remove other the higher fatty acid reactant of fusing point that swim in the rear liquid of reaction top, after reaction, liquid is cooled to room temperature, make modification oleic acid,
Oleic acid modification reaction equation is as follows:
CH
3(CH
2)
7CH=CH(CH
2)
7COOH+NaOHa→H
3(CH
2)
7CH=CH(CH
2)
7COONa+H
2O
The above-mentioned molecular formula that adds the product enuatrol of thermal response is C
18h
33naO
2; Its designs simplification is CH
3(CH
2)
7cH=CH (CH
2)
7cOONa, molecular weight 304.44.After having reacted according to aforesaid equation, sodium oleate solution concentration is about 2%, and reactant is soluble in water, has certain frothing capacity in water.
1:3~3.5, get respectively density 1.46g/cm in mass ratio
3sodium silicate and water, stir 15~20 minutes, form water glass solution; In adding the ratio of 3 kilograms of concentrated sulfuric acids in this water glass solution of double centner, the concentrated sulfuric acid is slowly added in water glass solution, stir 30~35 minutes, make acidified sodium silicate;
Step 2: fluorite ore raw ore is carried out to ore grinding, obtain the ore grinding ore pulp; By ore raw ore per ton join sodium carbonate 1200 grams, density is 1.46 g/cm
3the ratio of modification oleic acid 300 grams that make of sodium silicate 1500 grams, calgon 80 grams and step 1, the modification oleic acid that the sodium carbonate of corresponding weight, waterglass, calgon and step 1 are made adds in this ore grinding ore pulp, roughly selected at the temperature of 25~30 ℃, obtained roughly selecting foam and rougher tailings;
Step 3: join the ratio of the modification oleic acid that 100 gram steps 1 make in ore raw ore per ton, this modification oleic acid of corresponding weight is added in the rougher tailings of step 2, scanned;
The ratio of joining the modification oleic acid that acidified sodium silicate that 600 gram steps 1 make and 100 gram steps 1 make in ore raw ore per ton, this acidified sodium silicate of corresponding weight and this modification oleic acid are added respectively to roughly selecting in foam of step 2, carry out selected for the first time, selected foam for the first time;
Step 4: join the ratio of the acidified sodium silicate that 400 gram steps 1 make in ore raw ore per ton, this acidified sodium silicate of corresponding weight added in the selected foam for the first time of step 3, carry out selected for the second time, selected foam for the second time;
Step 5: join the ratio of the acidified sodium silicate that 200 gram steps 1 make in ore raw ore per ton, this acidified sodium silicate of corresponding weight added in the selected foam for the second time of step 4, carry out selected for the third time, selected foam for the third time;
Step 6: join the ratio of the acidified sodium silicate that 100 gram steps 1 make in ore raw ore per ton, this acidified sodium silicate of corresponding weight added in the selected foam for the third time of step 5, carry out the 4th time selected, obtain selected foam the 4th time;
Step 7: by existing technique to the 4th selected foam carry out successively the 5th time selected, the 6th time selected and the 7th time selected, make fluorite concentrate.
Technique of the present invention has solved the technical barrier of fluorite mineral and quartz and the sorting of calcite mineral.Adopt modification oleic acid as collecting agent, because modification oleic acid has good dissolubility in water, be easy to disperse, increased the chance that the modified oil acid molecule contacts with the purpose mineral, its consumption is relatively less, has formed selective collecting effect.And while adopting oleic acid to do collecting agent, because the oleic acid freezing point is high, solubility under normal temperature in water is extremely low, in the time of slurry temperature must being heated to 35~40 ℃, just can reach increase oleic acid in ore pulp solubility, improve oleic acid molecular dispersive property purpose in ore pulp, and oleic acid viscosity is larger, even if take to heat, its dispersiveness in ore pulp of measure of ore pulp is still poor, needs larger consumption competence exertion collecting effect, but has reduced selective collecting performance.Adopt modification oleic acid to reduce significantly the requirement of flotation to slurry temperature, also reduced collector dosage, reduced gangue mineral and be mingled with and enter fluorite concentrate.Add calgon, acidified sodium silicate composite restrainer at flotation operation, when coarse scan is elected to be industry, the inhibitory action of strengthening to gangue minerals such as quartz and calcites, improved the rough concentrate quality simultaneously; Reduce mash acid alkalinity when selected operation, increase the floatability difference between mineral, realize efficiently separating of calcirm-fluoride mineral and silica, calcium carbonate, reduce the content that enters selected operation gangue mineral, the use of composite restrainer, guaranteed the raising of fluorite concentrate grade and the higher sorting rate of recovery.Can obtain qualified acid level fluorite concentrate by technique of the present invention, recovery rate in ore-dressing is higher.
Add acidified sodium silicate in the selected operation of technique of the present invention, can reduce the acid-base value of ore pulp, increase the floatability difference between mineral, realize efficiently separating of calcirm-fluoride mineral and silica, calcium carbonate.
Technological adaptability of the present invention is strong, good stability, and the fluorite concentrate high-quality of output, the rate of recovery is high, and the ore dressing processing cost is low, and environmental pollution is less.
embodiment 1
1:340 in mass ratio, get respectively NaOH and water, be made into sodium hydroxide solution, pass into steam, make the temperature of this sodium hydroxide solution rise to 100 ℃, in adding the ratio of 1 kilogram of oleic acid in 53 kg of hydrogen sodium hydroxide solution, oleic acid is added in the sodium hydroxide solution after intensification, stir 30 minutes, react fully and carry out, continue to pass into steam in the process that adds oleic acid and stir in sodium hydroxide solution, make reaction temperature remain at 100 ℃, after adding thermal response and completing, stop adding steam, standing 30 minutes, remove other the higher fatty acid reactant of fusing point that swim in the rear liquid of reaction top, after reaction, liquid is cooled to room temperature, make modification oleic acid, 1:3, be 1.46g/cm by density in mass ratio
3sodium silicate be added to the water, stir 15 minutes, form water glass solution, in adding the ratio of 3 kilograms of concentrated sulfuric acids in this water glass solution of double centner, the concentrated sulfuric acid is slowly added in water glass solution, stir 30 minutes, make acidified sodium silicate, by the technological process shown in Fig. 1, the fluorite ore ore of Calcium Fluoride Content 60%, dioxide-containing silica 20%, calcium carbonate content 15% is carried out to ore grinding, obtain the ore grinding ore pulp, fluorite ore raw ore is carried out to ore grinding, obtain the ore grinding ore pulp, by ore raw ore per ton join sodium carbonate 1200 grams, density is 1.46 g/cm
3sodium silicate 1500 grams, calgon 80 grams and the ratio of modification oleic acid 300 grams that make, the sodium carbonate of corresponding weight, waterglass, calgon and the modification oleic acid that makes are added in this ore grinding ore pulp, roughly selected at the temperature of 30 ℃, obtained roughly selecting foam and rougher tailings, in ore raw ore per ton join 100 restrain the ratio of modification oleic acid, this modification oleic acid of corresponding weight is added in rougher tailings, scanned,
In ore raw ore per ton join 600 restrain acidified sodium silicate and 100 restrain the ratio of modification oleic acid, the acidified sodium silicate of corresponding weight and modification oleic acid are added respectively and roughly select in foam, carry out selected for the first time, selected foam for the first time; In ore raw ore per ton join 400 restrain the ratio of acidified sodium silicate, this acidified sodium silicate of corresponding weight is added for the first time in selected foam, carry out selected for the second time, selected foam for the second time; In ore raw ore per ton join 200 restrain the ratio of acidified sodium silicate, this acidified sodium silicate of corresponding weight is added for the second time in selected foam, carry out selected for the third time, selected foam for the third time; In ore raw ore per ton join 100 restrain the ratio of acidified sodium silicate, this acidified sodium silicate of corresponding weight is added for the third time in selected foam, carry out the 4th time selected, obtain selected foam the 4th time; By existing technique to the 4th selected foam carry out successively the 5th time selected, the 6th time selected and the 7th time selected, make fluorite concentrate.
Detect by analysis, the sorting index of this fluorite concentrate is: fluorinated calcium 97.54%, silica 1 .06%, calcium carbonate 0.95%, the calcirm-fluoride rate of recovery is 90.51%, as shown in table 1.
The sorting index of the fluorite concentrate that table 1 adopts ore-dressing technique of the present invention to obtain
comparative Examples 1
Conventional ore-dressing technique shown in employing Fig. 2 is carried out ore dressing to the fluorite ore ore of Calcium Fluoride Content 60%, dioxide-containing silica 20%, calcium carbonate content 15%, and slurry temperature during flotation is 35 ℃~40 ℃, makes fluorite concentrate.Detect by analysis, the sorting index of this fluorite concentrate is: fluorite concentrate fluorinated calcium 95.81%, silica 1 .41%, calcium carbonate 2.46%, in fluorite concentrate, the calcirm-fluoride rate of recovery is 90.08%, as shown in table 2.
The sorting index of the fluorite concentrate that the conventional ore-dressing technique of table 2 obtains
As can be seen from Table 1 and Table 2: at complicated difficult, select in the ore dressing process of fluorite ore, ore-dressing technique of the present invention has been improved flotation efficiency, has improved fluorite concentrate ore deposit grade and the rate of recovery, has effectively reduced the content of silica and calcium carbonate in the fluorite concentrate.This is that sodium carbonate is the soda acid adjusting agent because ore-dressing technique of the present invention has adopted modification oleic acid to do collecting agent, and acidified sodium silicate and calgon composite restrainer, form selective collecting, selective inhibitory.
embodiment 2
1:350 in mass ratio, get respectively NaOH and water, be made into sodium hydroxide solution, pass into steam, make the temperature of this sodium hydroxide solution rise to 90 ℃, in adding the ratio of 1 kilogram of oleic acid in 53 kg of hydrogen sodium hydroxide solution, oleic acid is added in the sodium hydroxide solution after intensification, stir 35 minutes, react fully and carry out, continue to pass into steam in the process that adds oleic acid and stir in sodium hydroxide solution, make reaction temperature remain at 90 ℃, after adding thermal response and completing, stop passing into steam, standing 40 minutes, remove other the higher fatty acid reactant of fusing point that swim in the rear liquid of reaction top, after reaction, liquid is cooled to room temperature, make modification oleic acid, 1:3.5, be 1.46g/cm by density in mass ratio
3sodium silicate be added to the water, stir 20 minutes, form water glass solution, in adding the ratio of 3 kilograms of concentrated sulfuric acids in this water glass solution of double centner, the concentrated sulfuric acid is slowly added in water glass solution, stir 35 minutes, make acidified sodium silicate.Fluorite ore ore raw ore to Calcium Fluoride Content 48%, dioxide-containing silica 34%, calcium carbonate content 16% carries out ore grinding, obtains the ore grinding ore pulp; By ore raw ore per ton join sodium carbonate 1200 grams, density is 1.46g/cm
3sodium silicate 1500 grams, calgon 80 grams and the ratio of modification oleic acid 300 grams that make, the sodium carbonate of corresponding weight, waterglass, calgon and the modification oleic acid that makes are added in this ore grinding ore pulp, roughly selected at the temperature of 29 ℃, obtained roughly selecting foam and rougher tailings; In ore raw ore per ton join 100 restrain the ratio of modification oleic acid, this modification oleic acid of corresponding weight is added in rougher tailings, scanned; In ore raw ore per ton join 600 restrain acidified sodium silicate and 100 restrain the ratio of modification oleic acid, this acidified sodium silicate of corresponding weight and this modification oleic acid are added and roughly select in foam, carry out selected for the first time, selected foam for the first time; In ore raw ore per ton join 400 restrain the ratio of acidified sodium silicate, this acidified sodium silicate of corresponding weight is added for the first time in selected foam, carry out selected for the second time, selected foam for the second time; In ore raw ore per ton join 200 restrain the ratio of acidified sodium silicate, this acidified sodium silicate of corresponding weight is added for the second time in selected foam, carry out selected for the third time, selected foam for the third time; In ore raw ore per ton join 100 restrain the ratio of acidified sodium silicate, this acidified sodium silicate of corresponding weight is added for the third time in selected foam, carry out the 4th time selected, obtain selected foam the 4th time; By existing technique to the 4th selected foam carry out successively the 5th time selected, the 6th time selected and the 7th time selected, make fluorite concentrate.
The sorting index of this fluorite concentrate is: fluorite concentrate fluorinated calcium grade 97.73%, silica 0.78%, calcium carbonate 0.67%, in fluorite concentrate, the calcirm-fluoride rate of recovery is 81.15%.
comparative Examples 2
The conventional ore-dressing technique of employing Fig. 2 is carried out ore dressing to the fluorite ore ore of Calcium Fluoride Content 48%, dioxide-containing silica 34%, calcium carbonate content 16%, and slurry temperature during ore dressing is 35 ℃~40 ℃, obtains fluorite concentrate.The sorting index of this fluorite concentrate is: fluorite concentrate fluorinated calcium grade 97.38%, silica 1 .91%, calcium carbonate 1.87%, in fluorite concentrate, the calcirm-fluoride rate of recovery is 76.93%.
By embodiment 2 and Comparative Examples 2, can find out, when adopting technique of the present invention identical complicated difficult selecting fluorite ore to carry out ore dressing to component content respectively with common process, the calcirm-fluoride rate of recovery of technique of the present invention is higher than the calcirm-fluoride rate of recovery of common process; And in the fluorite concentrate that obtains of technique ore dressing of the present invention, the content of silica and calcium carbonate all is less than the content of silica and calcium carbonate in the fluorite concentrate that the common process ore dressing obtains, the fluorite concentrate that ore-dressing technique of the present invention obtains has reached the quality requirement of sour level fluorite concentrate seconds.
embodiment 3
1:345 in mass ratio, get respectively NaOH and water, be made into sodium hydroxide solution, pass into steam, make the temperature of this sodium hydroxide solution rise to 95 ℃, in adding the ratio of 1 kilogram of oleic acid in 53 kg of hydrogen sodium hydroxide solution, oleic acid is added in the sodium hydroxide solution after intensification, stir 32 minutes, react fully and carry out, continue to pass into steam in the process that adds oleic acid and stir in sodium hydroxide solution, make reaction temperature remain at 95 ℃, after adding thermal response and completing, stop passing into steam, standing 50 minutes, remove other the higher fatty acid reactant of fusing point that swim in the rear liquid of reaction top, after reaction, liquid is cooled to room temperature, make modification oleic acid, 1:3.25, be 1.46g/cm by density in mass ratio
3sodium silicate be added to the water, stir 18 minutes, form water glass solution, in adding the ratio of 3 kilograms of concentrated sulfuric acids in this water glass solution of double centner, the concentrated sulfuric acid is slowly added in water glass solution, stir 34 minutes, make acidified sodium silicate, fluorite ore raw ore is carried out to ore grinding, obtain the ore grinding ore pulp, by ore raw ore per ton join sodium carbonate 1200 grams, density is 1.46g/cm
3sodium silicate 1500 grams, calgon 80 grams and the ratio of modification oleic acid 300 grams that make, the sodium carbonate of corresponding weight, waterglass, calgon and the modification oleic acid that makes are added in this ore grinding ore pulp, roughly selected at the temperature of 25 ℃, obtained roughly selecting foam and rougher tailings, in ore raw ore per ton join 100 restrain the ratio of modification oleic acid, this modification oleic acid of corresponding weight is added in rougher tailings, scanned, in ore raw ore per ton join 600 restrain acidified sodium silicate and 100 restrain the ratio of modification oleic acid, this acidified sodium silicate of corresponding weight and this modification oleic acid are added respectively and roughly select in foam, carry out selected for the first time, selected foam for the first time, in ore raw ore per ton join 400 restrain the ratio of acidified sodium silicate, this acidified sodium silicate of corresponding weight is added for the first time in selected foam, carry out selected for the second time, selected foam for the second time, in ore raw ore per ton join 200 restrain the ratio of acidified sodium silicate, this acidified sodium silicate of corresponding weight is added for the second time in selected foam, carry out selected for the third time, selected foam for the third time, in ore raw ore per ton join 100 restrain the ratio of acidified sodium silicate, this acidified sodium silicate of corresponding weight is added for the third time in selected foam, carry out the 4th time selected, obtain selected foam the 4th time, by existing technique to the 4th selected foam carry out successively the 5th time selected, the 6th time selected and the 7th time selected, make fluorite concentrate.
embodiment 4
1:342 in mass ratio, get respectively NaOH and water, be made into sodium hydroxide solution, pass into steam, make the temperature of this sodium hydroxide solution rise to 92 ℃, in adding the ratio of 1 kilogram of oleic acid in 53 kg of hydrogen sodium hydroxide solution, oleic acid is added in the sodium hydroxide solution after intensification, stir 34 minutes, react fully and carry out, continue to pass into steam in the process that adds oleic acid and stir in sodium hydroxide solution, make reaction temperature remain at 92 ℃, after adding thermal response and completing, stop passing into steam, standing 60 minutes, remove other the higher fatty acid reactant of fusing point that swim in the rear liquid of reaction top, after reaction, liquid is cooled to room temperature, make modification oleic acid, 1:3.1, be 1.46g/cm by density in mass ratio
3sodium silicate be added to the water, stir 16 minutes, form water glass solution, in adding the ratio of 3 kilograms of concentrated sulfuric acids in this water glass solution of double centner, the concentrated sulfuric acid is slowly added in water glass solution, stir 32 minutes, make acidified sodium silicate, fluorite ore raw ore is carried out to ore grinding, obtain the ore grinding ore pulp, by ore raw ore per ton join sodium carbonate 1200 grams, density is 1.46 g/cm
3sodium silicate 1500 grams, calgon 80 grams and the ratio of modification oleic acid 300 grams that make, the sodium carbonate of corresponding weight, waterglass, calgon and the modification oleic acid that makes are added in this ore grinding ore pulp, roughly selected at the temperature of 26 ℃, obtained roughly selecting foam and rougher tailings, in ore raw ore per ton join 100 restrain the ratio of modification oleic acid, this modification oleic acid of corresponding weight is added in rougher tailings, scanned, in ore raw ore per ton join 600 restrain acidified sodium silicate and 100 restrain the ratio of modification oleic acid, this acidified sodium silicate of corresponding weight and this modification oleic acid are added respectively and roughly select in foam, carry out selected for the first time, selected foam for the first time, in ore raw ore per ton join 400 restrain the ratio of acidified sodium silicate, this acidified sodium silicate of corresponding weight is added for the first time in selected foam, carry out selected for the second time, selected foam for the second time, in ore raw ore per ton join 200 restrain the ratio of acidified sodium silicate, this acidified sodium silicate of corresponding weight is added for the second time in selected foam, carry out selected for the third time, selected foam for the third time, in ore raw ore per ton join 100 restrain the ratio of acidified sodium silicate, this acidified sodium silicate of corresponding weight is added for the third time in selected foam, carry out the 4th time selected, obtain selected foam the 4th time, by existing technique to the 4th selected foam carry out successively the 5th time selected, the 6th time selected and the 7th time selected, make fluorite concentrate.
embodiment 5
1:348 in mass ratio, get respectively NaOH and water, be made into sodium hydroxide solution, pass into steam, make the temperature of this sodium hydroxide solution rise to 98 ℃, in adding the ratio of 1 kilogram of oleic acid in 53 kg of hydrogen sodium hydroxide solution, oleic acid is added in the sodium hydroxide solution after intensification, stir 33 minutes, react fully and carry out, continue to pass into steam in the process that adds oleic acid and stir in sodium hydroxide solution, make reaction temperature remain at 98 ℃, after adding thermal response and completing, stop passing into steam, standing 35 minutes, remove other the higher fatty acid reactant of fusing point that swim in the rear liquid of reaction top, after reaction, liquid is cooled to room temperature, make modification oleic acid, 1:3.4, be 1.46 g/cm by density in mass ratio
3sodium silicate be added to the water, stir 19 minutes, form water glass solution, in adding the ratio of 3 kilograms of concentrated sulfuric acids in this water glass solution of double centner, the concentrated sulfuric acid is slowly added in water glass solution, stir 33 minutes, make acidified sodium silicate, fluorite ore raw ore is carried out to ore grinding, obtain the ore grinding ore pulp, by ore raw ore per ton join sodium carbonate 1200 grams, density is 1.46 g/cm
3sodium silicate 1500 grams, calgon 80 grams and the ratio of modification oleic acid 300 grams that make, the sodium carbonate of corresponding weight, waterglass, calgon and the modification oleic acid that makes are added in this ore grinding ore pulp, roughly selected at the temperature of 27 ℃, obtained roughly selecting foam and rougher tailings, in ore raw ore per ton join 100 restrain the ratio of modification oleic acid, this modification oleic acid of corresponding weight is added in rougher tailings, scanned, in ore raw ore per ton join 600 restrain acidified sodium silicate and 100 restrain the ratio of modification oleic acid, this acidified sodium silicate of corresponding weight and this modification oleic acid are added respectively and roughly select in foam, carry out selected for the first time, selected foam for the first time, in ore raw ore per ton join 400 restrain the ratio of acidified sodium silicate, this acidified sodium silicate of corresponding weight is added for the first time in selected foam, carry out selected for the second time, selected foam for the second time, in ore raw ore per ton join 200 restrain the ratio of acidified sodium silicate, this acidified sodium silicate of corresponding weight is added for the second time in selected foam, carry out selected for the third time, selected foam for the third time, in ore raw ore per ton join 100 restrain the ratio of acidified sodium silicate, this acidified sodium silicate of corresponding weight is added for the third time in selected foam, carry out the 4th time selected, obtain selected foam the 4th time, by existing technique to the 4th selected foam carry out successively the 5th time selected, the 6th time selected and the 7th time selected, make fluorite concentrate.
Fluorite ore ore-dressing technique of the present invention can increase the efficiency of separation of calcirm-fluoride and silica and calcite, improves quality and the rate of recovery of fluorite concentrate, obtains high-quality acid level fluorite concentrate, has successfully solved the problem of complicated fluorite flotation difficulty.At complicated difficult, select the effect in the fluorite ore ore dressing remarkable, there is repeatability, the mineral processing index ideal.Simultaneously, reduce the requirement of fluorite mineral floating to slurry temperature, reduced energy resource consumption; Reduce the consumption of collecting agent oleic acid, reduced a large amount of oleic acid waste water that contains and effluxed the environmental pollution caused, there is economic benefit and social benefit preferably.
Claims (6)
1. a complicated difficult selects the fluorite ore ore-dressing technique, it is characterized in that, specifically carries out according to the following steps:
Step 1: in adding the ratio of 1 kilogram of oleic acid in 53 kg of hydrogen sodium hydroxide solution, oleic acid is added to the sodium hydroxide solution that temperature is 90 ℃~100 ℃, and stir, react fully and carry out, standing after, remove other fatty acid reactant, be cooled to room temperature, make modification oleic acid;
In adding the ratio of 3 kilograms of concentrated sulfuric acids in the double centner water glass solution, the concentrated sulfuric acid is added in water glass solution, stir, make acidified sodium silicate;
Step 2: the fluorite ore raw ore is carried out to ore grinding, obtain the ore grinding ore pulp; By ore raw ore per ton join sodium carbonate 1200 grams, density is 1.46 g/cm
3the ratio of modification oleic acid 300 grams that make of sodium silicate 1500 grams, calgon 80 grams and step 1, the modification oleic acid that the sodium carbonate of corresponding weight, sodium silicate, calgon and step 1 are made adds in this ore grinding ore pulp, roughly selected at the temperature of 25 ℃~30 ℃, obtained roughly selecting foam and rougher tailings;
Step 3: join the ratio of the modification oleic acid that 100 gram steps 1 make in ore raw ore per ton, this modification oleic acid of corresponding weight is added in the rougher tailings of step 2, scanned;
The ratio of joining the modification oleic acid that acidified sodium silicate that 600 gram steps 1 make and 100 gram steps 1 make in ore raw ore per ton, this acidified sodium silicate of corresponding weight and this modification oleic acid are added respectively to roughly selecting in foam of step 2, carry out selected for the first time, selected foam for the first time;
Step 4: join the ratio of the acidified sodium silicate that 400 gram steps 1 make in ore raw ore per ton, this acidified sodium silicate of corresponding weight added in the selected foam for the first time of step 3, carry out selected for the second time, selected foam for the second time;
Step 5: join the ratio of the acidified sodium silicate that 200 gram steps 1 make in ore raw ore per ton, this acidified sodium silicate of corresponding weight added in the selected foam for the second time of step 4, carry out selected for the third time, selected foam for the third time;
Step 6: join the ratio of the acidified sodium silicate that 100 gram steps 1 make in ore raw ore per ton, this acidified sodium silicate of corresponding weight added in the selected foam for the third time of step 5, carry out the 4th time selected, obtain selected foam the 4th time;
Step 7: by existing technique to the 4th selected foam carry out successively the 5th time selected, the 6th time selected and the 7th time selected, make fluorite concentrate.
2. complicated difficult as claimed in claim 1 selects the fluorite ore ore-dressing technique, it is characterized in that, NaOH and water that in described step 1, sodium hydroxide solution used is 1:340~350 by mass ratio are formulated.
3. complicated difficult as claimed in claim 1 selects the fluorite ore ore-dressing technique, it is characterized in that, in described step 1, oleic acid adds sodium hydroxide solution, stirs temperature-resistant in this Hydrogen sodium hydroxide solution 30 minutes ~ 35 minutes.
4. complicated difficult as claimed in claim 1 selects the fluorite ore ore-dressing technique, it is characterized in that, in described step 1, and after sufficient reacting carries out, standing at least 30 minutes, remove other fatty acid reactant, be cooled to room temperature, make modification oleic acid.
5. complicated difficult as claimed in claim 1 selects the fluorite ore ore-dressing technique, it is characterized in that, the preparation of water glass solution in described step 1: 1:3~3.5 in mass ratio are 1.46g/cm by density
3waterglass be added to the water, stir 15 minutes~20 minutes, make water glass solution.
6. complicated difficult as claimed in claim 1 selects the fluorite ore ore-dressing technique, it is characterized in that, in described step 1, adds water glass solution to stir 25 minutes ~ 30 minutes the concentrated sulfuric acid.
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