CN109607527B - Beneficiation and purification method of low-grade microcrystalline graphite - Google Patents
Beneficiation and purification method of low-grade microcrystalline graphite Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
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- 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
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Abstract
The invention relates to a beneficiation and purification method of low-grade microcrystalline graphite, which comprises the steps of crushing and grinding raw microcrystalline graphite ore in sequence, adding a collecting agent and a foaming agent into ore pulp after grinding, stirring, and carrying out graphite flotation to obtain rough graphite concentrate and tailings 1; carrying out primary concentration and primary scavenging on the rough graphite concentrate to obtain concentrated concentrate and tailings 2; carrying out primary regrinding and concentration on the concentrated concentrate to obtain primary regrinding concentrated concentrate and primary regrinding concentrated tailings; and (3) regrinding the first regrinding and selecting concentrate for 1-2 times, and then performing concentration for 2-4 times under an acidic condition to obtain high-grade graphite concentrate and regrinding tailings. The beneficiation and purification method has the advantages of short flow and high enrichment ratio, solves the problems of low technical index, low graphite concentrate grade, low recovery rate, complex process and high cost of low-grade aphanitic graphite beneficiation, and enables low-grade microcrystalline graphite to be efficiently, economically and reasonably utilized.
Description
Technical Field
The invention relates to a beneficiation and purification method of low-grade microcrystalline graphite, and belongs to the technical field of beneficiation.
Background
Graphite is a non-metallic mineral material and raw material with excellent performance and wide application, and is widely applied to industrial departments of metallurgy, chemical industry, new energy automobiles, mechanical equipment, electronic information, nuclear power, aerospace, national defense and the like. China is rich in graphite resources and is the country with the largest natural graphite reserves, yields and exports in the world. Microcrystalline graphite, commonly known as "earthy graphite", has a crystal diameter of less than 1 μm and a specific surface area of 1-5m2The fixed carbon content of raw ore is generally 40-80% between/g, and a small amount is more than 90%, and quartz, dolomite, calcite, mica, kaolin and the like are associated with the raw ore. Although the fixed carbon content of the raw ore is high, the embedded particle size is extremely fine, and high-grade graphite products are difficult to select by the conventional process. At present, the microcrystalline graphite is mainly used as low-grade coal to be added into coal for sale at low price, and a very small amount of microcrystalline graphite is used as a low-end steel carburant after being simply crushed, heated and dried, so that precious graphite resources are seriously wasted. Therefore, research and development of a beneficiation method for recovering low-grade microcrystalline graphite are urgently needed.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a beneficiation and purification method of low-grade microcrystalline graphite, and the method is used for solving the technical problems of low grade and low recovery rate of graphite concentrate obtained by beneficiation and purification of the existing microcrystalline graphite ore.
In order to solve the technical problems, the technical scheme of the invention is as follows: a mineral separation and purification method of low-grade microcrystalline graphite comprises the following steps:
(1) sequentially crushing and grinding the microcrystalline graphite raw ore to ensure that the content of the ground ore with the fineness of-0.074 mm is 65-75%;
(2) adding a collecting agent and a foaming agent into the ore pulp obtained in the step (1) after ore grinding, stirring for 1-2 minutes, and performing graphite flotation to obtain graphite rough concentrate and tailings 1;
(3) carrying out primary concentration and primary scavenging on the rough graphite concentrate obtained in the step (2) to obtain concentrated concentrate and tailings 2;
(4) performing primary regrinding and concentration on the concentrated concentrate obtained in the step (3) to obtain primary regrinding concentrated concentrate and primary regrinding concentrated tailings;
(5) and (4) regrinding the reground concentrate obtained in the step (4) for 1-2 times, and then carrying out concentration for 2-4 times under an acidic condition to obtain high-grade graphite concentrate and reground tailings.
Further, in the step (1), the microcrystalline graphite raw ore is crushed to-3 mm and then ground.
Further, in the step (2), the graphite flotation process comprises 1-2 times of roughing and 0-1 time of scavenging, wherein the concentration of the roughed ore pulp is 15-20wt%, and the flotation time is 2-6 min.
Further, in the step (2) and the step (3), the using amount of the collecting agent is 100-500 g/ton and the using amount of the foaming agent is 50-100 g/ton during rough concentration; during scavenging, the using amount of the collecting agent is 20-50 g/ton, and the using amount of the foaming agent is 0-30 g/ton; during concentration, the dosage of the collecting agent is 10-30 g/ton, and the dosage of the foaming agent is 0-10 g/ton.
Further, in the step (4), the selected concentrate is reground for the first time, so that the regrinding concentration is 30-35wt%, and the content of the grinded ore with the fineness of-0.037 mm is 85-90%; adding a collecting agent and a foaming agent, and performing 1-2 concentration with concentration of 10-15wt% to obtain first reground concentrate and first reground tailings; wherein the dosage of the collecting agent is 10-30 g/ton, and the dosage of the foaming agent is 5-10 g/ton.
Further, in the step (5), the first regrinding concentrated concentrate is reground for the second time, so that the concentration of the regrinding for the second time is 30-35wt%, and the content of the grinding ore with the fineness of-0.037 mm is 90-95%; adjusting the pH value of the ore pulp to 3-4, adding 10-30 g/ton of collecting agent and 5-10 g/ton of foaming agent, and carrying out concentration for 1 time, wherein the concentration of concentration is 5-10wt%, so as to obtain second regrinding concentrate and second regrinding tailings; carrying out third regrinding on the second regrinding and fine-selecting concentrate to ensure that the regrinding concentration is 25-30wt%, the grinding fineness is-0.037 mm, the content is 95-99%, and the pH value of the ore pulp is adjusted to 3-4; then 10-20 g/ton of collecting agent and 5-10 g/ton of foaming agent are added for 1 time of concentration, the concentration of concentration is 2-5wt%, and high-grade graphite concentrate and third regrinding concentration tailings are obtained.
Further, combining the first regrinding concentration tailings, the second regrinding concentration tailings and the third regrinding concentration tailings for recleaning, and adding a collecting agent and a foaming agent, wherein the flotation concentration is 5-10wt%, and middling flotation concentrate and tailings 3 are obtained, wherein the using amount of the collecting agent is 30-60 g/ton, and the using amount of the foaming agent is 10-20 g/ton.
Further, the middling flotation concentrate is returned to step (3) for further processing.
Further, the collector comprises emulsified kerosene.
Further, the blowing agent includes an ethyl ether alcohol. The ether alcohol bubble performance is moderate, and the flotation effect is improved. Compared with the traditional terpineol foaming agent, the high-solubility high-molecular-weight polyether polyol has higher solubility, larger molecular weight entering the solution and more excellent bubble capacity, so that the probability of collision and adhesion of bubbles and target minerals is higher, the consumption of the agent is reduced, and the graphite product obtained by using ether alcohols as the foaming agent has higher recovery rate.
Further, the fixed carbon content in the microcrystalline graphite raw ore is lower than 60%.
In the invention, the regrinding and cleaning concentrate is cleaned under an acid condition, on one hand, the graphite has better acid resistance and corrosion resistance, the floatability of the graphite does not change under the acid condition, and gangue minerals such as quartz, dolomite, calcite and the like in the graphite concentrate are easy to generate compounds and volatile matters which are dissolved in water under the acid condition, thereby achieving the purpose of purifying the graphite; on the other hand, the acidic mineral system can eliminate the disturbance of inevitable ions such as calcium, magnesium, iron and the like.
The beneficiation and purification method has the advantages of short flow and high enrichment ratio, solves the problems of low technical index, low grade of graphite concentrate, low recovery rate, complex process and high cost of low-grade aphanitic graphite beneficiation, and ensures that the fixed carbon content and the recovery rate of the obtained microcrystal graphite flotation concentrate product can reach more than 90 percent, so that the low-grade microcrystal graphite ore is efficiently, economically and reasonably utilized.
Drawings
Figure 1 is a schematic flow diagram of a beneficiation process used in an embodiment of the present invention.
Detailed Description
Example 1
The fixed carbon content of the microcrystalline graphite ore in Hunan is 55.32wt%, the ore mainly comprises graphite, gangue minerals such as mica, quartz and chlorite, and a small amount of montmorillonite and calcite. The small amount of metal sulfide minerals are pyrite, blende, galena and chalcopyrite, respectively. In addition, it contains a small amount of apatite, rutile, etc.
Under the condition of grinding fineness of 72.18%, adding 400 g/ton of collecting agent emulsified kerosene and 80 g/ton of foaming agent ethyl ether alcohol into raw ore, and performing primary roughing to obtain roughed concentrate and tailings 1; the roughing concentrate is subjected to primary concentration to obtain a concentrating concentrate and tailings 2; carrying out primary regrinding on the selected concentrate, wherein the regrinding concentration is 28%, the content of grinding fineness of-0.037 mm is 88%, the dosage of emulsified kerosene is 30 g/ton, the dosage of ethyl ether alcohol is 10 g/ton, carrying out 2-time fine selection, and the concentration of fine selection is 12%, thus obtaining primary regrinding selected concentrate and primary regrinding selected tailings; the first regrinding concentration concentrate is reground for the second time, the regrinding concentration for the second time is 32%, the grinding fineness is-0.037 mm, the content of the grinding ore is 90%, the pH value of the ore pulp is adjusted to be 3.5, the dosage of emulsified kerosene is 20 g/ton, the dosage of ethyl ether alcohol is 5 g/ton, 1-time concentration is carried out, the concentration of concentration is 6%, and the regrinding concentration concentrate for the second time and the regrinding concentration tailing for the second time are prepared; and (3) carrying out third regrinding on the secondary regrinding and selecting concentrate, wherein the regrinding concentration is 27%, the grinding fineness is 94% of minus 0.037mm, the pH value of the ore pulp is adjusted to be 3, then adding 10 g/ton of emulsified kerosene and 5 g/ton of ethyl ether alcohol, carrying out 1-time selection, and the selection concentration is 3%, thus obtaining high-grade graphite concentrate and third regrinding and selecting tailings. And combining the first regrinding concentration tailings, the second regrinding concentration tailings and the third regrinding concentration tailings, regrinding and recleaning to obtain recleaning concentrate and tailings 3. Example 1 the results of the test are shown in table 1. The fixed carbon content of the obtained graphite concentrate is 90.17%, and the recovery rate reaches 90.12%.
Table 1 example 1 test results (%)
Example 2
The raw ore is selected from microcrystalline graphite ore of Heilongjiang, the fixed carbon content in the ore is 44.92wt%, the main mineral in the ore is graphite, and the main gangue mineral is quartz, illite and muscovite.
Under the condition of 66.98% grinding fineness of raw ore, 350 g/ton of collecting agent emulsified kerosene and 50 g/ton of foaming agent ethyl ether alcohol are added, and rough concentration and tailings 1 are obtained through one-time rough concentration; the roughing concentrate is subjected to primary concentration to obtain a concentrating concentrate and tailings 2; carrying out primary regrinding on the selected concentrate, wherein the regrinding concentration is 30%, the content of grinding fineness of 0.037mm is 85%, the dosage of emulsified kerosene is 30 g/ton, the dosage of ethyl ether alcohol is 10 g/ton, carrying out 2-time fine selection, and the concentration of fine selection is 10%, thus obtaining primary regrinding selected concentrate and primary regrinding selected tailings; carrying out secondary regrinding on the first regrinding and selecting concentrate, wherein the regrinding concentration of the secondary regrinding is 28%, the grinding fineness is-0.037 mm, the content of the grinding ore is 92%, adjusting the pH value of the ore pulp to be 3.5, adding 20 g/ton of emulsified kerosene and 5 g/ton of ethyl ether alcohol, carrying out 1-time selection, and the selection concentration is 5% to prepare secondary regrinding and selecting concentrate and secondary regrinding and selecting tailings; and (3) carrying out third regrinding on the secondary regrinding and selecting concentrate, wherein the regrinding concentration is 25%, the grinding fineness is 95% with the content of minus 0.037mm, the pH value of the ore pulp is adjusted to be 3, then adding 10 g/ton of emulsified kerosene and 5 g/ton of ethyl ether alcohol, carrying out 1-time selection, and the selection concentration is 2%, thus obtaining high-grade graphite concentrate and third regrinding and selecting tailings. And combining the first regrinding concentration tailings, the second regrinding concentration tailings and the third regrinding concentration tailings, regrinding and recleaning to obtain recleaning concentrate and tailings 3.
Example 2 the test results are shown in table 2. The fixed carbon content of the obtained graphite concentrate is 90.33%, and the recovery rate reaches 90.15%.
Table 2 example 2 test results (%)
The foregoing examples are set forth to illustrate the present invention more clearly and are not to be construed as limiting the scope of the invention, which is defined in the appended claims to which the invention pertains, as modified in all equivalent forms, by those skilled in the art after reading the present invention.
Claims (6)
1. The beneficiation and purification method of the low-grade microcrystalline graphite is characterized by comprising the following steps:
(1) sequentially crushing and grinding the microcrystalline graphite raw ore to ensure that the content of the ground ore with the fineness of-0.074 mm is 65-75%;
(2) adding a collecting agent and a foaming agent into the ore pulp obtained in the step (1) after ore grinding, stirring for 1-2min, and performing graphite flotation to obtain graphite rough concentrate and tailings 1;
the collecting agent is emulsified kerosene, and the foaming agent is ethyl ether alcohol;
(3) carrying out primary concentration and primary scavenging on the rough graphite concentrate obtained in the step (2) to obtain concentrated concentrate and tailings 2;
(4) performing primary regrinding and concentration on the concentrated concentrate obtained in the step (3) to obtain primary regrinding concentrated concentrate and primary regrinding concentrated tailings;
(5) carrying out regrinding on the primary regrinding and concentrating concentrate obtained in the step (4) for 2 times, and then carrying out concentration for 2 times under an acidic condition to obtain high-grade graphite concentrate and regrinding tailings;
wherein, in the step (4), the selected concentrate is reground for the first time, so that the regrind concentration is 30-35wt%, and the content of the grinding fineness of-0.037 mm is 85-90%; adding a collecting agent and a foaming agent, and performing 1-2 concentration with concentration of 10-15wt% to obtain first reground concentrate and first reground tailings; wherein the dosage of the collecting agent is 10-30 g/ton, and the dosage of the foaming agent is 5-10 g/ton;
in the step (5), the first regrinding concentrated concentrate is reground for the second time, so that the regrinding concentration for the second time is 30-35wt%, and the content of the grinded ore with the fineness of-0.037 mm is 90-95%; adjusting the pH value of the ore pulp to 3-4, adding 10-30 g/ton of collecting agent and 5-10 g/ton of foaming agent, and carrying out concentration for 1 time, wherein the concentration of concentration is 5-10wt%, so as to obtain second regrinding concentrate and second regrinding tailings; carrying out third regrinding on the second regrinding and fine-selecting concentrate to ensure that the regrinding concentration is 25-30wt%, the grinding fineness is-0.037 mm, the content is 95-99%, and the pH value of the ore pulp is adjusted to 3-4; then 10-20 g/ton of collecting agent and 5-10 g/ton of foaming agent are added for 1 time of concentration, the concentration of concentration is 2-5wt%, and high-grade graphite concentrate and third regrinding concentration tailings are obtained.
2. The beneficiation purification method according to claim 1, wherein in the step (1), the raw microcrystalline graphite ore is crushed to-3 mm and ground.
3. The beneficiation purification method according to claim 1, wherein in the step (2), the graphite flotation process comprises 1-2 times of roughing and 0-1 times of scavenging, wherein the concentration of the rougher pulp is 15-20wt%, and the flotation time is 2-6 min.
4. The beneficiation purification method according to claim 1, wherein in the step (2) and the step (3), the amount of the collecting agent is 100-500 g/ton, and the amount of the foaming agent is 50-100 g/ton; during scavenging, the using amount of the collecting agent is 20-50 g/ton, and the using amount of the foaming agent is 0-30 g/ton; during concentration, the dosage of the collecting agent is 10-30 g/ton, and the dosage of the foaming agent is 0-10 g/ton.
5. The mineral processing purification method of claim 1, wherein the first reground concentration tailings, the second reground concentration tailings and the third reground concentration tailings are combined for recleaning, and a collector and a foaming agent are added, wherein the flotation concentration is 5-10wt%, and middling flotation concentrate and tailings 3 are obtained, wherein the amount of the collector is 30-60 g/ton, and the amount of the foaming agent is 10-20 g/ton.
6. The beneficiation purification method according to claim 5, wherein the middling flotation concentrate is returned to step (3) for further processing.
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| CN110395726B (en) * | 2019-09-04 | 2021-03-16 | 湖南有色金属研究院 | Purification method of microcrystalline graphite ore |
| CN112387424A (en) * | 2020-10-23 | 2021-02-23 | 湖南有色金属研究院 | Flotation separation method of microcrystalline graphite and sulfide ore |
| CN112642583A (en) * | 2020-12-29 | 2021-04-13 | 黑龙江省宝泉岭农垦溢祥石墨有限公司 | Graphite flotation middling treatment process and device |
| CN114308373B (en) * | 2022-01-06 | 2022-10-21 | 中国地质大学（北京） | Method for utilizing graphite ore full resources |
| CN114853005B (en) * | 2022-06-20 | 2024-03-29 | 苏州中材非金属矿工业设计研究院有限公司 | Short-process purification method for graphite by combined separation of machine and column |
| CN115043399B (en) * | 2022-07-26 | 2023-06-30 | 中国矿业大学(北京) | Method for efficiently purifying coal-based graphite |
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