CN112387424A - Flotation separation method of microcrystalline graphite and sulfide ore - Google Patents

Flotation separation method of microcrystalline graphite and sulfide ore Download PDF

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Publication number
CN112387424A
CN112387424A CN202011151940.2A CN202011151940A CN112387424A CN 112387424 A CN112387424 A CN 112387424A CN 202011151940 A CN202011151940 A CN 202011151940A CN 112387424 A CN112387424 A CN 112387424A
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China
Prior art keywords
graphite
flotation
microcrystalline graphite
ore
microcrystalline
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曾惠明
陈代雄
杨建文
胡波
朱雅卓
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Hunan Research Institute of Non Ferrous Metals
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Hunan Research Institute of Non Ferrous Metals
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/001Flotation agents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/02Froth-flotation processes
    • B03D1/025Froth-flotation processes adapted for the flotation of fines
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00Specified effects produced by the flotation agents
    • B03D2201/007Modifying reagents for adjusting pH or conductivity
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00Specified effects produced by the flotation agents
    • B03D2201/02Collectors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2203/00Specified materials treated by the flotation agents; specified applications
    • B03D2203/02Ores

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Abstract

The invention provides a flotation separation method of microcrystalline graphite and sulfide ore, which comprises the following steps: crushing raw ore, and performing ball milling to obtain 60-95% microcrystalline graphite ore powder with the fineness of-0.074 mm; adding water into the microcrystalline graphite mineral powder and stirring to obtain microcrystalline graphite ore pulp, wherein the concentration of the ore pulp is 8-15%; and after rough concentration operation and scavenging operation are sequentially carried out on the microcrystalline graphite ore pulp, rough graphite concentrate and tailings are obtained, the tailings are discarded, and after regrinding operation and pulping are carried out on the rough graphite concentrate, fine concentration operation is carried out to obtain the microcrystalline graphite concentrate. The method adopts the green and environment-friendly flotation reagent, has small pollution and light environmental pressure, can improve the flotation separation efficiency of the microcrystalline graphite and the sulphide ore to more than 94 percent, and realizes the flotation purification of the microcrystalline graphite with low cost and high efficiency on the premise of green and environment protection.

Description

Flotation separation method of microcrystalline graphite and sulfide ore
Technical Field
The invention relates to the field of mineral processing, in particular to a flotation separation method of microcrystalline graphite and sulfide ore.
Background
Graphite is an important strategic resource, has excellent performance and very wide application, and has very large market demand in the future. The microcrystalline graphite with large resource reserve and high raw ore grade belongs to one of graphite resources, and has the characteristics of good electrical and thermal conductivity, isotropy and the like. Abundant microcrystalline graphite resources are reserved in Hunan province, and the method has very high economic value and good development and application prospects. However, the crystal size of the microcrystalline graphite exceeds the flotation lower limit, and the raw ore contains impurities such as sulfide ore, mica and the like with good floatability, so that the flotation and purification of the microcrystalline graphite are always difficult in ore dressing.
The mineral composition of the microcrystalline graphite ore mainly comprises graphite, a small amount of gangue minerals, mainly mica and quartz, and a small amount of metal sulfide minerals, mainly pyrite, and secondly zinc blende, galena, chalcopyrite and the like. Therefore, the essence of the flotation and purification of the microcrystalline graphite ore is the separation of graphite from gangue and sulfide minerals. Compared with the flotation separation of gangue minerals and graphite, the pyrite-based sulfide minerals have better surface hydrophobicity and floatability, and are more difficult to separate from microcrystalline graphite by flotation. And because the conventional flotation for inhibiting sulfide ores such as pyrite and the like is generally carried out under the condition of high alkalinity (adding a large amount of lime), the environmental pollution is great.
Therefore, it is necessary to provide a method for separating microcrystalline graphite by flotation, which can improve the separation efficiency of microcrystalline graphite and sulfide ore with good floatability on the premise of environmental protection.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a flotation separation method of microcrystalline graphite and sulphide ore, aiming at improving the separation efficiency of the microcrystalline graphite and sulphide ore with good floatability and solving the technical problem of difficult flotation separation of the microcrystalline graphite and sulphide ore in the flotation purification process of the microcrystalline graphite ore on the premise of environmental protection.
In order to achieve the aim, the invention provides a flotation separation method of microcrystalline graphite and sulphide ore, which comprises the following steps:
s1, grinding: crushing raw ore, and performing ball milling to obtain 60-95% microcrystalline graphite ore powder with the fineness of-0.074 mm;
s2, pulping: adding water into the microcrystalline graphite mineral powder and stirring to obtain microcrystalline graphite ore pulp, wherein the concentration of the ore pulp is 8-15%;
s3, flotation: the microcrystalline graphite ore pulp is subjected to roughing operation and scavenging operation in sequence to obtain graphite rough concentrate and tailings, the tailings are discarded, and the graphite rough concentrate is subjected to regrinding operation and pulping and then is subjected to concentration operation to obtain microcrystalline graphite concentrate; flotation regulators and flotation collectors are sequentially added in the roughing operation and the concentrating operation to float the microcrystalline graphite minerals, and only the flotation collectors are added in the scavenging operation;
the flotation regulator is etherified starch, the adding amount in each roughing operation is 100-2000 g/t, the stirring time after adding is 1-5 min, the adding amount in each refining operation is 10-300 g/t, and the stirring time after adding is 1-5 min; the flotation collector is MA, and the MA is composed of 60-70 parts of kerosene and 20-30 parts of ether alcohol by weight; the adding amount of MA in each roughing operation is 50-500g/t, the stirring time after adding is 1-5 min, the adding amount of MA in each scavenging operation is 10-300 g/t, the stirring time after adding is 1-5 min, the adding amount of MA in each refining operation is 10-300 g/t, and the stirring time after adding is 1-5 min.
Preferably, the graphite rough concentrate with the thickness of 0.037mm accounts for 90-98% after regrinding operation in the step (3), and the pulp concentration after pulping is 8-12%.
Preferably, in the step (3), the number of roughing operation is 1-2, the number of scavenging operation is 1-3, the number of regrinding operation is 1-3, and the number of fine selection operation is 3-6.
The microcrystalline graphite belongs to graphite with very tiny crystals, the surface of the graphite is nonpolar and has good natural hydrophobicity, and the sulfide ore mainly containing pyrite is a polar surface and has good hydrophobicity under the action of a collecting agent. The etherified starch forms a stable colloidal solution in a pulp system, and the medicament molecule has a hydrophilic functional group (alkyl) and a hydrophilic functional group (hydroxyl) after being hydrolyzed, and has a strong inhibiting effect on sulfide ore. After certain etherified starch is added into the ore pulp, the hydrophilic group of the etherified starch can act with the surface of sulfide minerals, so that the sulfide minerals in the ore pulp have hydrophilic performance and reduced floatability, and the microcrystalline graphite on the non-polar surface does not act with CMS (sodium carboxymethyl cellulose), thereby realizing the flotation separation of the microcrystalline graphite and the sulfide minerals.
The invention has the beneficial effects that: the method adopts the green and environment-friendly flotation reagent, has small pollution and light environmental pressure, can improve the flotation separation efficiency of the microcrystalline graphite and the sulphide ore to more than 94 percent, and realizes the flotation purification of the microcrystalline graphite with low cost and high efficiency on the premise of green and environment protection.
Drawings
FIG. 1 is a schematic flow diagram of a flotation separation process of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the accompanying drawings and specific embodiments.
Aiming at the existing problems, the invention provides a flotation separation method of microcrystalline graphite and sulphide ore, which comprises the following steps: crushing raw ore, and performing ball milling to obtain 60-95% microcrystalline graphite ore powder with the fineness of-0.074 mm; adding water into the microcrystalline graphite mineral powder and stirring to obtain microcrystalline graphite ore pulp, wherein the concentration of the ore pulp is 8-15%; the microcrystalline graphite ore pulp is subjected to roughing operation and scavenging operation in sequence to obtain graphite rough concentrate and tailings, the tailings are discarded, and the graphite rough concentrate is subjected to regrinding operation and pulping and then is subjected to concentration operation to obtain microcrystalline graphite concentrate; flotation regulators and flotation collectors are sequentially added in the roughing operation and the concentrating operation to float microcrystalline graphite minerals, and only the flotation collectors are added in the scavenging operation
The flotation regulator is etherified starch, the adding amount in each roughing operation is 100-2000 g/t, the stirring time after adding is 1-5 min, the adding amount in each refining operation is 10-300 g/t, and the stirring time after adding is 1-5 min; the flotation collector is MA, and the MA is composed of 60-70 parts of kerosene and 20-30 parts of 3-benzyloxy benzyl alcohol by weight; the adding amount of MA in each roughing operation is 50-500g/t, the stirring time after adding is 1-5 min, the adding amount of MA in each scavenging operation is 10-300 g/t, the stirring time after adding is 1-5 min, the adding amount of MA in each refining operation is 10-300 g/t, and the stirring time after adding is 1-5 min.
Wherein, the graphite rough concentrate with the thickness of 0.037mm accounts for 90-95% after the regrinding operation in the step (3), and the pulp concentration after pulping is 8-12%; in the step (3), the number of roughing operation is 1-2, the number of scavenging operation is 1-3, the number of regrinding operation is 1-3, and the number of fine selection operation is 3-6.
Example 1
The preparation method comprises the steps of selecting Shandong pond microcrystalline graphite ore in Chenzhou, Hunan, and detecting that the fixed carbon content in raw ore is 68.50%, the sulfur content is 0.75%, the raw ore mainly comprises graphite, and the metal minerals comprise pyrite, hematite and trace chalcopyrite; the gangue with high mineral content is quartz, muscovite, biotite, etc. Because the embedded particle size of the microcrystalline graphite is fine, and the sulfide ore, the gangue and the graphite are interwoven and intergrown, the flotation and purification difficulty of the microcrystalline graphite ore is very high, and the specific operation steps of the embodiment are as follows:
(1) grinding: crushing raw ore, and performing ball milling to obtain 78% microcrystalline graphite ore powder with the fineness of-0.074 mm;
(2) pulping: adding water into the microcrystalline graphite mineral powder and stirring to obtain microcrystalline graphite pulp, wherein the pulp concentration is 12%;
(3) flotation: the flotation operation comprises one roughing, one scavenging and four times of fine selection, wherein 500g/t of inhibitor carboxymethyl starch sodium is added in the roughing operation, the mixture is stirred for 3min, 200g/t of MA is added, the mixture is stirred for 1min, and the flotation time is 5 min; adding 50g/t of MA in the scavenging operation, stirring for 2min, wherein the flotation time is 4min, obtaining rough graphite concentrate and tailings after the scavenging operation, and discarding the tailings. And (2) regrinding the rough graphite concentrate, wherein the fineness of reground ore grinding is 92-0.037 mm, the ore pulp concentration is 10%, then carrying out flotation concentration, wherein the flotation concentration operation is four times of concentration, 200g/t of sodium carboxymethyl starch and 20g/t of MA are added in the first concentration, 100g/t of sodium carboxymethyl starch and 20g/t of MA are added in the second concentration, 100g/t of sodium carboxymethyl starch and 10g/t of MA are added in the third concentration, and 100g/t of sodium carboxymethyl starch and 10g/t of MA are added in the fourth concentration, so that the graphite concentrate is obtained.
After the flotation graphite concentrate is dried, the fixed carbon content is 90.50 percent, the sulfur content is 0.06 percent, the separation efficiency of the microcrystalline graphite and the sulfide ore exceeds 94 percent, and the efficient flotation separation of the microcrystalline graphite ore and the sulfide ore is realized.
Example 2
Selecting the same raw ore as the raw ore in the embodiment 1, and specifically operating the following steps:
(1) grinding: crushing raw ore, and performing ball milling to obtain microcrystalline graphite ore powder with the fineness of-0.074 mm accounting for 80%;
(2) pulping: adding water into the microcrystalline graphite mineral powder and stirring to obtain microcrystalline graphite pulp, wherein the pulp concentration is 10%;
(3) flotation: the flotation operation comprises secondary roughing, primary scavenging and five-time fine selection, wherein 500g/t of inhibitor etherified starch is added in the first roughing operation, stirring is carried out for 3min, 50g/t of MA is added, stirring is carried out for 1min, and the flotation time is 5 min; adding 300g/t of inhibitor etherified starch, stirring for 3min, adding 20g/t of MA, stirring for 1min, and floating for 4 min; adding 200g/t of MA in the first scavenging operation, stirring for 3min, wherein the flotation time is 3min, adding 20g/t of MA in the second scavenging operation, stirring for 1min, and performing flotation for 3 min; and (4) obtaining rough graphite concentrate and tailings after scavenging operation, and discarding the tailings. And (2) regrinding the rough graphite concentrate, wherein the fineness of reground ore grinding is 95-0.037 mm, the ore pulp concentration is 8%, then performing flotation concentration, wherein the flotation concentration operation is five times of concentration, 200g/t of etherified starch and 20g/t of MA are added in the first concentration, 200g/t of etherified starch and 20g/t of MA are added in the second concentration, 200g/t of etherified starch and 20g/t of MA are added in the third concentration, 100g/t of etherified starch and 10g/t of MA are added in the fourth concentration, and 100g/t of etherified starch and 10g/t of MA are added in the fifth concentration, so that the graphite concentrate is obtained.
After drying treatment, the flotation graphite concentrate is detected to have fixed carbon content of 91.50 percent and sulfur content of 0.04 percent, the separation efficiency of the microcrystalline graphite and the sulfide ore exceeds 95 percent, and the efficient flotation separation of the microcrystalline graphite and the sulfide ore is realized.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (3)

1. A flotation separation method of microcrystalline graphite and sulfide ore is characterized by comprising the following steps:
s1, grinding: crushing raw ore, and performing ball milling to obtain 60-95% microcrystalline graphite ore powder with the fineness of-0.074 mm;
s2, pulping: adding water into the microcrystalline graphite mineral powder and stirring to obtain microcrystalline graphite ore pulp, wherein the concentration of the ore pulp is 8-15%;
s3, flotation: the microcrystalline graphite ore pulp is subjected to roughing operation and scavenging operation in sequence to obtain graphite rough concentrate and tailings, the tailings are discarded, and the graphite rough concentrate is subjected to regrinding operation and pulping and then is subjected to concentration operation to obtain microcrystalline graphite concentrate; flotation regulators and flotation collectors are sequentially added in the roughing operation and the concentrating operation to float the microcrystalline graphite minerals, and only the flotation collectors are added in the scavenging operation;
the flotation regulator is etherified starch, the adding amount in each roughing operation is 100-2000 g/t, the stirring time after adding is 1-5 min, the adding amount in each refining operation is 10-300 g/t, and the stirring time after adding is 1-5 min; the flotation collector is MA, and the MA is composed of 60-70 parts of kerosene and 20-30 parts of ether alcohol by weight; the adding amount of MA in each roughing operation is 50-500g/t, the stirring time after adding is 1-5 min, the adding amount of MA in each scavenging operation is 10-300 g/t, the stirring time after adding is 1-5 min, the adding amount of MA in each refining operation is 10-300 g/t, and the stirring time after adding is 1-5 min.
2. The flotation separation method for microcrystalline graphite and sulphide ore according to claim 1, wherein the graphite rough concentrate after regrinding operation in step (3) is 0.037mm and accounts for 90-98%, and the pulp concentration after pulping is 8-12%.
3. The method for flotation separation of microcrystalline graphite and sulphide ore according to claim 1, wherein the number of roughing operations in step (3) is 1-2, the number of scavenging operations is 1-3, the number of regrinding operations is 1-3, and the number of concentrating operations is 3-6.
CN202011151940.2A 2020-10-23 2020-10-23 Flotation separation method of microcrystalline graphite and sulfide ore Pending CN112387424A (en)

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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101890398A (en) * 2010-07-12 2010-11-24 南通北极光自动控制技术有限公司 Multifunctional ore dressing chemical, synthesis method thereof and using method thereof
CN102580855A (en) * 2012-01-19 2012-07-18 西北有色地质研究院 Method for separating lead from carbon and copper in copper-lead-zinc mixed sulfide ore
CN104069952A (en) * 2014-06-06 2014-10-01 武汉理工大学 Inhibitor for gangue mineral in graphite ore and application thereof
CN105032622A (en) * 2015-09-04 2015-11-11 长春黄金研究院 Two-section synthesis method for beneficiation reagent
CN105197920A (en) * 2015-10-20 2015-12-30 辽宁工程技术大学 Microcrystal graphite separation and purification method
CN106622675A (en) * 2016-10-29 2017-05-10 广西佛子矿业有限公司 Preparing method of novel copper and lead flotation separation inhibitor FY09
CN107638949A (en) * 2017-09-29 2018-01-30 江西理工大学 Application of the cation etherification starch in Scheelite Flotation
CN109607527A (en) * 2017-12-05 2019-04-12 湖南有色金属研究院 A kind of purification by mineral method of low-grade micro crystal graphite
CN110465412A (en) * 2019-09-20 2019-11-19 栾川县秦豫科技有限公司 A kind of molybdenite beneficiation inhibitor and preparation method thereof

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101890398A (en) * 2010-07-12 2010-11-24 南通北极光自动控制技术有限公司 Multifunctional ore dressing chemical, synthesis method thereof and using method thereof
CN102580855A (en) * 2012-01-19 2012-07-18 西北有色地质研究院 Method for separating lead from carbon and copper in copper-lead-zinc mixed sulfide ore
CN104069952A (en) * 2014-06-06 2014-10-01 武汉理工大学 Inhibitor for gangue mineral in graphite ore and application thereof
CN105032622A (en) * 2015-09-04 2015-11-11 长春黄金研究院 Two-section synthesis method for beneficiation reagent
CN105197920A (en) * 2015-10-20 2015-12-30 辽宁工程技术大学 Microcrystal graphite separation and purification method
CN106622675A (en) * 2016-10-29 2017-05-10 广西佛子矿业有限公司 Preparing method of novel copper and lead flotation separation inhibitor FY09
CN107638949A (en) * 2017-09-29 2018-01-30 江西理工大学 Application of the cation etherification starch in Scheelite Flotation
CN109607527A (en) * 2017-12-05 2019-04-12 湖南有色金属研究院 A kind of purification by mineral method of low-grade micro crystal graphite
CN110465412A (en) * 2019-09-20 2019-11-19 栾川县秦豫科技有限公司 A kind of molybdenite beneficiation inhibitor and preparation method thereof

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Application publication date: 20210223