CN115318427A - Process and device for preparing nanoscale ultrapure carbon material by using coal slime - Google Patents
Process and device for preparing nanoscale ultrapure carbon material by using coal slime Download PDFInfo
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- 239000003245 coal Substances 0.000 title claims abstract description 116
- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 34
- 230000008569 process Effects 0.000 title claims abstract description 25
- 238000000227 grinding Methods 0.000 claims abstract description 104
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 64
- 238000000746 purification Methods 0.000 claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 238000010008 shearing Methods 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 238000003860 storage Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 7
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- 239000004088 foaming agent Substances 0.000 claims description 65
- 238000005188 flotation Methods 0.000 claims description 30
- 239000003350 kerosene Substances 0.000 claims description 27
- SJWFXCIHNDVPSH-UHFFFAOYSA-N octan-2-ol Chemical compound CCCCCCC(C)O SJWFXCIHNDVPSH-UHFFFAOYSA-N 0.000 claims description 22
- 238000005273 aeration Methods 0.000 claims description 18
- 239000012141 concentrate Substances 0.000 claims description 14
- 239000000919 ceramic Substances 0.000 claims description 11
- 238000007865 diluting Methods 0.000 claims description 11
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- 230000018044 dehydration Effects 0.000 claims description 10
- 238000006297 dehydration reaction Methods 0.000 claims description 10
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- 238000000926 separation method Methods 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 4
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- 239000003513 alkali Substances 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
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- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 10
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- RHZUVFJBSILHOK-UHFFFAOYSA-N anthracen-1-ylmethanolate Chemical compound C1=CC=C2C=C3C(C[O-])=CC=CC3=CC2=C1 RHZUVFJBSILHOK-UHFFFAOYSA-N 0.000 description 1
- 239000003830 anthracite Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
- B03B7/00—Combinations of wet processes or apparatus with other processes or apparatus, e.g. for dressing ores or garbage
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Abstract
The invention relates to the technical field of coal slime separation, in particular to a process and a device for preparing a nanoscale ultrapure carbon material by using coal slime. The production method specifically comprises the following steps: preparing raw ore pulp: putting the coal slime raw material into a feeding storage tank, and adding water to prepare raw ore pulp; roughing; fine selection; filtering; coarse grinding; fine grinding; shearing and stirring; primary purification; secondary purification; purifying for the third time; dehydrating and drying to obtain the nano-scale ultrapure carbon material, and putting the nano-scale ultrapure carbon material into a product warehouse for storage. The method can be used for directly and deeply deashing the coal slime to produce the ultrapure carbon material, can realize continuous operation, has good deashing effect, can reduce the ash content of a product to below 3 percent, completely avoids adding strong corrosion agents such as strong acid, strong alkali and the like, adopts a pure physical method, has simple equipment, safe and environment-friendly process, completely eliminates energy consumption required by high-temperature heating reaction in the chemical deashing process, has low energy consumption and stable product granularity, has high yield and stable deashing effect, and is suitable for large-scale production and application.
Description
Technical Field
The invention relates to the technical field of coal slime separation, in particular to a process and a device for preparing a nanoscale ultrapure carbon material by using coal slime.
Background
In actual production and application, the main means for reducing the ash content of the coal slime is flotation, but the method can only reduce the ash content to about 9 percent, and a chemical method is mostly adopted for deep deashing.
Although the Shenhua Ningxia coal industry group Taixi coal washing factory completes research and application of key technology for sorting ultra-low ash pure coal from broken and dissociated smokeless clean lump coal, and realizes production from lump clean coal to ultra-low ash pure coal, the ash content of the clean coal of the raw material Taixi coal lump is extremely low (generally, the ash content of coal slime is 6-8 times of the ash content of the clean coal of the Taixi coal lump), so the method is not suitable for other coal types, and deep deashing of other coal types still depends on a chemical method.
The chemical deliming is mainly formed by adding strong alkali and strong acid to react under a heating condition to dissolve ash, an ultrapure carbon material can be obtained after washing, filtering and other processes, the process flow is complex and has high requirements on equipment, and a chemical medium cannot be recycled, so that environmental pollution is easily caused.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art, and therefore, an aspect of the present invention is to provide a process and an apparatus for preparing a nano-scale ultrapure carbon material from coal slurry.
The production method specifically comprises the following steps:
s1, preparing raw ore pulp: putting the coal slime raw material into a feeding storage tank, adding water and preparing raw ore pulp;
s2, roughing: adding the raw ore pulp prepared in the S1 into a roughing flotation machine, and adding a foaming agent and a collecting agent for roughing to obtain roughing ore pulp;
s3, selection: adding the roughed pulp prepared in the step S2 into a fine flotation machine, and adding a foaming agent and a collecting agent for fine separation to obtain fine pulp;
s4, filtering: adding the selected ore pulp prepared in the step S3 into a disc filter for filtering to obtain concentrated ore concentrate;
s5, coarse grinding: adding the concentrated concentrate prepared in the step (S4) into a coarse grinding mill for coarse grinding to obtain coarse ground ore pulp;
s6, fine grinding: adding the coarse grinding ore pulp prepared in the step S5 into a fine grinding mill for fine grinding to obtain fine grinding ore pulp;
s7, shearing and stirring: adding the fine grinding ore pulp prepared in the step S6 into a shearing stirrer for stirring and adding water for diluting to obtain semi-finished ore pulp;
s8, primary purification: adding the semi-finished ore pulp prepared in the step S7 into a primary purifying machine, adding a foaming agent and a collecting agent, and carrying out primary purification to obtain primary purified ore pulp;
s9, secondary purification: adding the primary purified ore pulp prepared in the step S8 into a secondary purifying machine, adding water for dilution, adding a foaming agent and a collecting agent, and carrying out secondary purification to obtain secondary purified ore pulp;
s10, three-time purification: adding the secondary purified ore pulp prepared in the S9 into a tertiary purifying machine, adding water for dilution, adding a foaming agent and a collecting agent, and carrying out tertiary purification to obtain finished product ore pulp;
s11, dehydration and drying: and (4) adding the finished product ore pulp prepared in the step (S10) into a filter press for filter pressing and dehydration to prepare the nanoscale ultrapure carbon material, and putting the nanoscale ultrapure carbon material into a product warehouse for storage.
Preferably, the raw ore pulp in the S1 has the concentration of 70-90g/l and the granularity of coal slime particles is less than 0.5 mm.
Preferably, the foaming agent in the S2 and the S3 is sec-octanol, and the collecting agent is kerosene; the foaming agent is less than or equal to 300g/t of dry coal slime, and the collecting agent is less than or equal to 1000g/t of dry coal slime; the aeration quantity of the roughing flotation machine and the concentration flotation machine in the S2 and the S3 is 0.6-1.2m 3 /(m 2 Min) with the rotating speed of 350r/min; the ash content of the S2 roughing pulp is reduced to 12%; the S3 concentration pulp ash is reduced to 7%. The flotation machine consists of a motor IIIThe angle belt drives the impeller to rotate, so that a centrifugal effect is generated to form negative pressure, on one hand, sufficient air is sucked to be mixed with ore pulp, on the other hand, the ore pulp is stirred to be mixed with an additive, and meanwhile, foam is refined, so that mineral is bonded on the foam and floats to the surface of the ore pulp to form mineralized foam, the height of the flashboard is adjusted, the liquid level is controlled, and useful foam is scraped out by the scraper.
Preferably, the concentration of the concentrated concentrate in the S4 is 300-400g/l.
Preferably, in the step S5, the rotation speed of the coarse grinding mill is 72r/min, the coarse grinding time is 0.7h, the coarse grinding medium is ceramic balls, and the stage ratio of the coarse grinding medium is 20mm:15mm:12mm =3:4:3, obtaining the coarse grinding pulp with the granularity D90-45 μm.
Preferably, in the step S6, the rotation speed of the fine grinding mill is 160r/min, the fine grinding time is 0.3h, the coarse grinding medium is ceramic balls, and the number of the fine grinding medium is 5-6mm:3-4mm =1:1, the granularity of the obtained fine grinding ore pulp is more than or equal to 80 percent with minus 10 mu m.
Preferably, the stirring speed of the shear stirrer in the S7 is 100-200r/min, the stirring time is 5min, and the concentration of the semi-finished product ore pulp is 40-60g/l.
Preferably, the foaming agent in the S8 is sec-octanol, and the collecting agent is kerosene; the foaming agent is less than or equal to 300g/t of dry coal slime, and the collecting agent is less than or equal to 1000g/t of dry coal slime; the aeration quantity of the primary purifier is 0.6-1.2m 3 /(m 2 Min) and the rotating speed is 350r/min.
Preferably, the concentration of the primary purified ore pulp diluted by water in S9 is 20-30g/l; the foaming agent in the S9 is sec-octanol, and the collecting agent is kerosene; the foaming agent is less than or equal to 200g/t of dry coal slime, and the collecting agent is less than or equal to 800g/t of dry coal slime; the aeration rate of the secondary purification machine is 0.6-1.2m 3 /(m 2 Min) and the rotating speed is 350r/min.
Preferably, the concentration of the secondary purification ore pulp diluted by water in the S10 is 15-20g/l; the foaming agent in the S10 is sec-octanol, and the collecting agent is kerosene; the foaming agent has the weight ratio of less than or equal to 100g/t of dry coal slime, and the collecting agent has small weight ratioThe dry coal slime amount is equal to or more than 500g/t; the aeration quantity of the tertiary purifier is 0.6-1.2m 3 /(m 2 Min) and the rotating speed is 350r/min. The purifying machine and the flotation machine are the same and are driven by a motor triangle belt to rotate by a movable impeller to generate centrifugal action to form negative pressure, on one hand, sufficient air is sucked to be mixed with ore pulp, on the other hand, the ore pulp is stirred to be mixed with additives, meanwhile, foams are refined, minerals are enabled to be adhered to the foams, mineralized foams are formed after the foams float to the surface of the ore pulp, the height of a flashboard is adjusted, the liquid level is controlled, and useful foams are scraped out by a scraper blade.
Preferably, the pressure of the filter press in S11 is 7-10bar, and the ash content of the prepared nanoscale ultrapure carbon material is reduced to below 3%.
The invention has the following beneficial effects:
the invention creatively provides a grinding and floating process to carry out coal slime deep deliming, adds the grinding shearing and echelon deep deliming processes on the basis of the process for producing clean coal by coal slime flotation, and realizes the automatic, continuous and harmless production of deep deliming.
The method can be used for producing the ultrapure carbon material by directly and deeply deashing the coal slime, can realize continuous operation, has good deashing effect, can reduce the ash content of a product to below 3 percent, completely avoids adding strong corrosive agents such as strong acid, strong alkali and the like, adopts a pure physical method, has simple equipment, safe process and environmental protection, completely eliminates the energy consumption required by high-temperature heating reaction in the chemical deashing process, and has low energy consumption and stable product granularity.
The method is suitable for deashing of all coal slime, does not require the ash content of the coal slime, has high yield and stable deashing effect, does not change due to different ash contents of the coal slime, and is suitable for large-scale production and application.
The nano-scale ultrapure carbon material produced by the invention can be used as a raw material for producing cathode materials of sodium-ion batteries and lithium ion batteries, and simultaneously provides a raw material guarantee for researching and producing tip materials such as coal-based conductive materials, graphene, C/C composite materials and the like.
Additional aspects and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a schematic diagram of the connection of the apparatus of the present invention;
wherein: 1 is a feeding storage tank, 2 is a roughing flotation machine, 3 is a concentrating flotation machine, 4 is a disk filter, 5 is a rough grinding mill, 6 is a fine grinding mill, 7 is a shearing mixer, 8 is a primary purifier, 9 is a secondary purifier, 10 is a tertiary purifier, 11 is a filter press, and 12 is a product warehouse.
Detailed Description
In order that the above objects, features and advantages of the present invention can be more clearly understood, the present invention will be described in further detail with reference to the accompanying drawings and specific embodiments. It should be noted that the embodiments and features of the embodiments of the present application may be combined with each other without conflict.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced otherwise than as specifically described and, therefore, the scope of the present invention is not limited by the specific embodiments disclosed below.
Example one
Common coal slime with ash content of 36%, particle size of 0-0.5mm and concentration of 160-200g/l is selected and passed through the equipment shown in figure 1.
S1, preparing raw ore pulp: putting the coal slime raw material into a feeding storage tank 1, adding water to adjust the concentration of the raw ore pulp to be 80g/l, wherein the granularity of coal slime particles is below 0.5 mm;
s2, roughing: adding the raw ore pulp prepared in the step S1 into a rough flotation machine 2, wherein the aeration quantity of the rough flotation machine 2 is 1m 3 /(m 2 Min), the rotating speed is 350r/min, a foaming agent sec-octanol and a collecting agent kerosene are added, the weight ratio of the foaming agent is less than or equal to 300g/t of dry coal slime, the weight ratio of the collecting agent is less than or equal to 1000g/t of dry coal slime, and rough concentration is carried out to obtain rough concentration ore pulp;
s3, selection: adding the rougher pulp prepared in the step S2 into a fine flotation machine 3 for fine selectionThe aeration quantity of the flotation machine 3 is 1m 3 /(m 2 Min), the rotating speed is 350r/min, a foaming agent, namely octanol and a collecting agent, namely kerosene are added, the weight ratio of the foaming agent is less than or equal to 300g/t of dry coal slime, the weight ratio of the collecting agent is less than or equal to 1000g/t of dry coal slime, and concentration is carried out to obtain concentrated ore pulp;
s4, filtering: adding the selected ore pulp prepared in the S3 into a disc filter 4 for filtering to obtain concentrated concentrate with the concentration of 350g/l;
s5, coarse grinding: and (3) adding the concentrated concentrate prepared in the step (S4) into a coarse grinding mill 5 for coarse grinding, wherein the rotating speed of the coarse grinding mill 5 is 72r/min, the coarse grinding time is 0.7h, the coarse grinding medium is ceramic balls, and the series ratio of the coarse grinding medium is 20mm:15mm:12mm =3:4:3, obtaining coarse grinding ore pulp with the granularity D90-45 μm;
s6, fine grinding: adding the coarse grinding ore pulp prepared in the step S5 into a fine grinding mill 6 for fine grinding, wherein the rotating speed of the fine grinding mill 6 is 160r/min, the fine grinding time is 0.3h, the fine grinding medium is ceramic balls, and the series ratio of the fine grinding medium is 5-6mm:3-4mm =1:1, obtaining the refined pulp with the granularity of-10 mu m more than or equal to 80 percent;
s7, shearing and stirring: adding the refined pulp prepared in the step S6 into a shearing stirrer 7 for stirring at the stirring speed of 160r/min for 5min, adding water for dilution, and obtaining semi-finished pulp, wherein the concentration of the diluted pulp is 50g/l according to actual calculation;
s8, primary purification: adding the semi-finished ore pulp prepared in the step S7 into a primary purifier 8, adding a foaming agent sec-octanol and a collecting agent kerosene, wherein the weight ratio of the foaming agent is less than or equal to 300g/t of dry coal slime, the weight ratio of the collecting agent is less than or equal to 1000g/t of dry coal slime, and the air inflation amount of the primary purifier 8 is 1m 3 /(m 2 Min), the rotating speed is 350r/min, and primary purification is carried out to obtain primary purified ore pulp;
s9, secondary purification: adding the primary purified ore pulp prepared in the step S8 into a secondary purifier 9, diluting with water, wherein the diluted concentration of the water is 25g/l according to actual calculation, adding a foaming agent, namely secondary octanol and a collecting agent, namely kerosene, wherein the weight ratio of the foaming agent is less than or equal to 200g/t of dry coal slime, and the weight ratio of the collecting agent is less than or equal toThe dry coal slime amount is 800g/t, the aeration amount of the secondary purifier 9 is 1m 3 /(m 2 Min), the rotating speed is 350r/min, and secondary purification is carried out to obtain secondary purified ore pulp;
s10, three-time purification: adding the secondary purified ore pulp prepared in the step S9 into a tertiary purifier 10, diluting with water, wherein the diluted concentration of the water is 16g/l according to actual calculation, adding a foaming agent sec-octanol and a collecting agent kerosene, the weight ratio of the foaming agent is less than or equal to 100g/t of dry coal slime, the weight ratio of the collecting agent is less than or equal to 500g/t of dry coal slime, and the air inflation amount of the tertiary purifier 10 is 1m 3 /(m 2 Min), the rotating speed is 350r/min, and the finished product ore pulp is obtained through three times of purification;
s11, dehydration and drying: and (3) adding the finished product ore pulp prepared in the step (S10) into a filter press (11) for filter pressing dehydration, wherein the pressing pressure is 7bar, so that the nano-scale ultrapure carbon material is prepared, the yield is 9.35%, and the combustion detection ash content is 2.87.
Example two
Selecting anthracite coal slime of a new landscape mine in a Yangquan mining area, wherein the ash content is 32.08 percent, the particle size is less than 0.5mm, and the concentration is 160-200g/ll, and passing through equipment shown in figure 1.
S1, preparing raw ore pulp: putting the coal slime raw material into a feeding storage tank 1, adding water to adjust the concentration of the raw ore pulp to be 80g/l, wherein the granularity of coal slime particles is below 0.5 mm;
s2, roughing: adding the raw ore pulp prepared in the S1 into a rough flotation machine 2, wherein the aeration quantity of the rough flotation machine 2 is 1m 3 /(m 2 Min), the rotating speed is 350r/min, adding a foaming agent sec-octanol and a collecting agent kerosene, wherein the weight ratio of the foaming agent is less than or equal to 300g/t of dry coal slime, the weight ratio of the collecting agent is less than or equal to 1000g/t of dry coal slime, and performing rough separation to obtain rough separation ore pulp;
s3, selection: adding the rougher pulp prepared in the step S2 into a fine flotation machine 3, wherein the aeration quantity of the fine flotation machine 3 is 1m 3 /(m 2 Min), the rotating speed is 350r/min, a foaming agent, namely octanol and a collecting agent, namely kerosene are added, the weight ratio of the foaming agent is less than or equal to 300g/t of dry coal slime, the weight ratio of the collecting agent is less than or equal to 1000g/t of dry coal slime, and concentration is carried out to obtain concentrated ore pulp;
s4, filtering: adding the selected ore pulp prepared in the step S3 into a disc filter 4 for filtering to obtain concentrated ore concentrate with the concentration of 350g/l;
s5, coarse grinding: and (3) adding the concentrated concentrate prepared in the step (S4) into a coarse grinding mill 5 for coarse grinding, wherein the rotating speed of the coarse grinding mill 5 is 72r/min, the coarse grinding time is 0.7h, a coarse grinding medium is a ceramic ball, and the series ratio of the coarse grinding medium is 20mm:15mm:12mm =3:4:3, obtaining coarse grinding ore pulp with the granularity D90-45 μm;
s6, fine grinding: adding the coarse grinding ore pulp prepared in the step S5 into a fine grinding mill 6 for fine grinding, wherein the rotating speed of the fine grinding mill 6 is 160r/min, the fine grinding time is 0.3h, the fine grinding medium is ceramic balls, and the stage ratio of the fine grinding medium is 5-6mm:3-4mm =1:1, obtaining the fine grinding ore pulp with the granularity of-10 mu m more than or equal to 80 percent;
s7, shearing and stirring: adding the refined ore pulp prepared in the step S6 into a shearing stirrer 7 for stirring at the stirring speed of 160r/min for 5min, adding water for dilution, wherein the concentration of the diluted ore pulp is 50g/l according to actual calculation, and obtaining semi-finished ore pulp;
s8, primary purification: adding the semi-finished ore pulp prepared in the step S7 into a primary purifier 8, adding a foaming agent sec-octanol and a collecting agent kerosene, wherein the weight ratio of the foaming agent is less than or equal to 300g/t of dry coal slime, the weight ratio of the collecting agent is less than or equal to 1000g/t of dry coal slime, and the air inflation amount of the primary purifier 8 is 1m 3 /(m 2 Min), the rotating speed is 350r/min, and primary purification is carried out to obtain primary purified ore pulp;
s9, secondary purification: adding the primary purified ore pulp prepared in the step S8 into a secondary purifier 9, diluting with water, wherein the diluted concentration of the water is 25g/l according to actual calculation, adding a foaming agent sec-octanol and a collecting agent kerosene, the weight ratio of the foaming agent is less than or equal to 200g/t of dry coal slime, the weight ratio of the collecting agent is less than or equal to 800g/t of dry coal slime, and the air inflation amount of the secondary purifier 9 is 1m 3 /(m 2 Min), the rotating speed is 350r/min, and secondary purification is carried out to obtain secondary purified ore pulp;
s10, three-time purification: adding the secondary purified ore pulp prepared in the S9 into a tertiary purifier 10, and adding water for dilutionAdding water according to actual calculation, wherein the diluted concentration is 16g/l, adding a foaming agent, namely octanol and a collecting agent, namely kerosene, wherein the weight ratio of the foaming agent is less than or equal to 100g/t of dry coal slime, the weight ratio of the collecting agent is less than or equal to 500g/t of dry coal slime, and the air inflation amount of a tertiary purifier 10 is 1m 3 /(m 2 Min), the rotating speed is 350r/min, and the finished product ore pulp is obtained by three times of purification;
s11, dehydrating and drying: and (3) adding the finished product ore pulp prepared in the step (S10) into a filter press 11 for filter pressing dehydration, wherein the pressing pressure is 7bar, so that the nano-scale ultrapure carbon material is prepared, the yield is 12%, and the combustion detection ash content is 2.41.
TABLE 1 deashing comparison table for the first and second stages of the example
The method is suitable for most common coal slime, the coal slime of a new-landscape coal preparation plant is used as a comparison, under the same process parameters, the nano ultra-pure carbon material can be extracted from the common coal slime and the coal slime of the new-landscape coal preparation plant, the ash content is less than 3%, and the deliming effect is stable.
Comparative example 1
Common coal slime with ash content of 36%, particle size of 0-0.5mm and concentration of 160-200g/l is selected.
S1, preparing raw ore pulp: putting the coal slime raw material into a feeding storage tank 1, adding water to adjust the concentration of the raw ore pulp to be 80g/l, wherein the granularity of coal slime particles is below 0.5 mm;
s2, roughing: adding the raw ore pulp prepared in the step S1 into a rough flotation machine 2, wherein the aeration quantity of the rough flotation machine 2 is 1m 3 /(m 2 Min), the rotating speed is 350r/min, a foaming agent sec-octanol and a collecting agent kerosene are added, the weight ratio of the foaming agent is less than or equal to 300g/t of dry coal slime, the weight ratio of the collecting agent is less than or equal to 1000g/t of dry coal slime, and rough concentration is carried out to obtain rough concentration ore pulp;
s3, selection: adding the rougher pulp prepared in the step S2 into a fine flotation machine 3, wherein the aeration quantity of the fine flotation machine 3 is 1m 3 /(m 2 Min), rotation speed of 350r/min, additionThe method comprises the following steps of (1) carrying out concentration to obtain concentrated ore pulp, wherein a foaming agent is sec-octanol and a collecting agent is kerosene, the weight ratio of the foaming agent is less than or equal to 300g/t of dry coal slime, and the weight ratio of the collecting agent is less than or equal to 1000g/t of dry coal slime;
s4, filtering: adding the selected ore pulp prepared in the step S3 into a disc filter 4 for filtering to obtain concentrated ore concentrate with the concentration of 350g/l;
s5, coarse grinding: and (3) adding the concentrated concentrate prepared in the step (S4) into a coarse grinding mill 5 for coarse grinding, wherein the rotating speed of the coarse grinding mill 5 is 72r/min, the coarse grinding time is 0.7h, the coarse grinding medium is ceramic balls, and the series ratio of the coarse grinding medium is 20mm:15mm:12mm =3:4:3, obtaining coarse grinding ore pulp with the granularity D90-45 mu m;
s6, adding water for dilution: diluting the coarse grinding ore pulp prepared in the step S5 by adding water, wherein the concentration of diluted ore pulp is 50g/l according to actual calculation of the water adding amount, and thus semi-finished ore pulp is obtained;
s7, primary purification: adding the semi-finished ore pulp prepared in the step S6 into a primary purifier 8, adding a foaming agent sec-octanol and a collecting agent kerosene, wherein the weight ratio of the foaming agent is less than or equal to 300g/t of dry coal slime, the weight ratio of the collecting agent is less than or equal to 1000g/t of dry coal slime, and the air inflation amount of the primary purifier 8 is 1m 3 /(m 2 Min), the rotating speed is 350r/min, and primary purification is carried out to obtain primary purified ore pulp;
s8, secondary purification: adding the primary purified ore pulp prepared in the step S7 into a secondary purifier 9, diluting with water, wherein the diluted concentration of the water is 25g/l according to actual calculation, adding a foaming agent sec-octanol and a collecting agent kerosene, the weight ratio of the foaming agent is less than or equal to 200g/t of dry coal slime, the weight ratio of the collecting agent is less than or equal to 800g/t of dry coal slime, and the air inflation amount of the secondary purifier 9 is 1m 3 /(m 2 Min), the rotating speed is 350r/min, and secondary purification is carried out to obtain secondary purified ore pulp;
s9, three-time purification: adding the secondary purified ore pulp prepared in the step S8 into a tertiary purifier 10, diluting with water, wherein the diluted concentration of the water is 16g/l according to actual calculation, adding a foaming agent sec-octanol and a collecting agent kerosene, wherein the weight ratio of the foaming agent is less than or equal to 100g/t of dry coal slime, and the weight of the collecting agent is heavyThe weight ratio is less than or equal to 500g/t of dry coal slime, and the aeration quantity of the tertiary purifier 10 is 1m 3 /(m 2 Min), the rotating speed is 350r/min, and the finished product ore pulp is obtained through three times of purification;
s10, dewatering and drying: and (3) adding the finished product ore pulp prepared in the step (S9) into a filter press 11 for filter pressing dehydration, wherein the pressing pressure is 7bar, so that a carbon material is prepared, and the combustion detection ash content is 8.3%.
Comparative example No. two
Common coal slime with ash content of 36%, particle size of 0-0.5mm and concentration of 160-200g/l is selected.
S1, preparing raw ore pulp: putting the coal slime raw material into a feeding storage tank 1, adding water to adjust the concentration of the raw ore pulp to be 80g/l, wherein the granularity of coal slime particles is below 0.5 mm;
s2, roughing: adding the raw ore pulp prepared in the S1 into a rough flotation machine 2, wherein the aeration quantity of the rough flotation machine 2 is 1m 3 /(m 2 Min), the rotating speed is 350r/min, a foaming agent sec-octanol and a collecting agent kerosene are added, the weight ratio of the foaming agent is less than or equal to 300g/t of dry coal slime, the weight ratio of the collecting agent is less than or equal to 1000g/t of dry coal slime, and rough concentration is carried out to obtain rough concentration ore pulp;
s3, selection: adding the rougher pulp prepared in the step S2 into a fine flotation machine 3, wherein the aeration quantity of the fine flotation machine 3 is 1m 3 /(m 2 Min), the rotating speed is 350r/min, a foaming agent, namely octanol and a collecting agent, namely kerosene are added, the weight ratio of the foaming agent is less than or equal to 300g/t of dry coal slime, the weight ratio of the collecting agent is less than or equal to 1000g/t of dry coal slime, and concentration is carried out to obtain concentrated ore pulp;
s4, filtering: adding the selected ore pulp prepared in the S3 into a disc filter 4 for filtering to obtain concentrated concentrate with the concentration of 350g/l;
s5, coarse grinding: and (3) adding the concentrated concentrate prepared in the step (S4) into a coarse grinding mill 5 for coarse grinding, wherein the rotating speed of the coarse grinding mill 5 is 72r/min, the coarse grinding time is 0.7h, the coarse grinding medium is ceramic balls, and the series ratio of the coarse grinding medium is 20mm:15mm:12mm =3:4:3, obtaining coarse grinding ore pulp with the granularity D90-45 μm;
s6, fine grinding: adding the coarse grinding ore pulp prepared in the step S5 into a fine grinding mill 6 for fine grinding, wherein the rotating speed of the fine grinding mill 6 is 160r/min, the fine grinding time is 0.3h, the fine grinding medium is ceramic balls, and the series ratio of the fine grinding medium is 5-6mm:3-4mm =1:1, obtaining the refined pulp with the granularity of-10 mu m more than or equal to 80 percent;
s7, shearing and stirring: adding the refined pulp prepared in the step S6 into a shearing stirrer 7 for stirring at the stirring speed of 160r/min for 5min, adding water for dilution, and obtaining semi-finished pulp, wherein the concentration of the diluted pulp is 50g/l according to actual calculation;
s8, primary purification: adding the semi-finished ore pulp prepared in the step S7 into a primary purifier 8, adding a foaming agent sec-octanol and a collecting agent kerosene, wherein the weight ratio of the foaming agent is less than or equal to 300g/t of dry coal slime, the weight ratio of the collecting agent is less than or equal to 1000g/t of dry coal slime, and the air inflation amount of the primary purifier 8 is 1m 3 /(m 2 Min), the rotating speed is 350r/min, and primary purification is carried out to obtain primary purified ore pulp;
s9, secondary purification: adding the primary purified ore pulp prepared in the step S8 into a secondary purifying machine 9, diluting with water, wherein the diluted concentration of the added water amount is 25g/l according to actual calculation, adding a foaming agent sec-octanol and a collecting agent kerosene, wherein the weight ratio of the foaming agent is less than or equal to 200g/t of dry coal slime, the weight ratio of the foaming agent is less than or equal to 800g/t of dry coal slime, and the air charge of the secondary purifying machine 9 is 1m 3 /(m 2 Min), the rotating speed is 350r/min, and secondary purification is carried out to obtain finished product ore pulp;
s10, dehydration and drying: and (3) adding the finished product ore pulp prepared in the step (S9) into a filter press 11 for filter pressing dehydration, wherein the pressing pressure is 7bar, so that a carbon material is prepared, and the ash content is 3.22% in combustion detection.
In the case that the raw materials and the data are the same, the first comparative example reduces the steps of fine grinding and shearing stirring, and the second comparative example reduces the steps of three times of purification, so that the ash content of the obtained carbon material is high and the particle size is large. It is further proved that the process steps of the invention are all but one absent in order to prepare the nano-scale ultrapure carbon material with good deliming effect.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and it is obvious to those skilled in the art that various modifications and variations can be made in the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A process and a device for preparing a nanoscale ultrapure carbon material by using coal slime are characterized in that: the production method specifically comprises the following steps:
s1, preparing raw ore pulp: putting the coal slime raw material into a feeding storage tank (1), and adding water to prepare raw ore pulp;
s2, roughing: adding the raw ore pulp prepared in the step S1 into a roughing flotation machine (2), and adding a foaming agent and a collecting agent for roughing to obtain roughing ore pulp;
s3, selection: adding the roughed pulp prepared in the S2 into a fine flotation machine (3), and adding a foaming agent and a collecting agent for fine selection to obtain fine pulp;
s4, filtering: adding the selected ore pulp prepared in the step S3 into a disc filter (4) for filtering to obtain concentrated ore concentrate;
s5, coarse grinding: adding the concentrated concentrate prepared in the step S4 into a coarse grinding mill (5) for coarse grinding to obtain coarse grinding ore pulp;
s6, fine grinding: adding the coarse grinding ore pulp prepared in the step S5 into a fine grinding mill (6) for fine grinding to obtain fine grinding ore pulp;
s7, shearing and stirring: adding the fine grinding ore pulp prepared in the step S6 into a shearing stirrer (7) for stirring and adding water for diluting to obtain semi-finished ore pulp;
s8, primary purification: adding the semi-finished ore pulp prepared in the step S7 into a primary purifying machine (8), adding a foaming agent and a collecting agent, and carrying out primary purification to obtain primary purified ore pulp;
s9, secondary purification: adding the primary purified ore pulp prepared in the step S8 into a secondary purifying machine (9), diluting with water, adding a collecting agent and a foaming agent, and performing secondary purification to obtain secondary purified ore pulp;
s10, three-time purification: adding the secondary purified ore pulp prepared in the S9 into a tertiary purifying machine (10), diluting with water, adding a foaming agent and a collecting agent, and carrying out tertiary purification to obtain finished ore pulp;
s11, dehydration and drying: and (3) adding the finished product ore pulp prepared in the step (S10) into a filter press (11) for filter pressing and dehydration to prepare the nano-scale ultrapure carbon material, and storing the nano-scale ultrapure carbon material in a product warehouse (12).
2. The process and apparatus for preparing nano-scale ultrapure carbon material using coal slime as claimed in claim 1, wherein: the concentration of the raw ore pulp in the S1 is 70-90g/l, and the granularity of coal slime particles is below 0.5 mm.
3. The process and apparatus for preparing nano-scale ultrapure carbon material from coal slime according to claim 1, wherein: the foaming agent in the S2 and the S3 is sec-octanol, and the collecting agent is kerosene; the foaming agent is less than or equal to 300g/t of dry coal slime, and the collecting agent is less than or equal to 1000g/t of dry coal slime; the aeration quantity of the roughing flotation machine (2) and the concentration flotation machine (3) in the S2 and the S3 is 0.6-1.2m 3 /(m 2 Min) with the rotating speed of 350r/min; the ash content of the S2 roughing pulp is reduced to 12%; the S3 concentration pulp ash is reduced to 7%.
4. The process and apparatus for preparing nano-scale ultrapure carbon material using coal slime as claimed in claim 1, wherein: and the concentration of the concentrated concentrate in the S4 is 300-400g/l.
5. The process and apparatus for preparing nano-scale ultrapure carbon material using coal slime as claimed in claim 1, wherein: in the S5, the rotating speed of the coarse grinding mill (5) is 72r/min, the coarse grinding time is 0.7h, the coarse grinding medium is ceramic balls, and the stage ratio of the coarse grinding medium is 20mm:15mm:12mm =3:4:3, obtaining the coarse grinding pulp with the granularity D90-45 μm.
6. The process and apparatus for preparing nano-scale ultrapure carbon material from coal slime according to claim 1, wherein: in the S6, the rotation speed of the fine grinding mill (6) is 160r/min, the fine grinding time is 0.3h, the fine grinding medium is ceramic balls, and the stage ratio of the fine grinding medium is 5-6mm:3-4mm =1:1, the granularity of the obtained fine grinding ore pulp is more than or equal to 80 percent with minus 10 mu m.
7. The process and apparatus for preparing nano-scale ultrapure carbon material using coal slime as claimed in claim 1, wherein: and in the S7, the stirring speed of the shearing stirrer (7) is 100-200r/min, the stirring time is 5min, and the concentration of the semi-finished ore pulp is 40-60g/l.
8. The process and apparatus for preparing nano-scale ultrapure carbon material using coal slime as claimed in claim 1, wherein: the foaming agent in the S8 is sec-octanol, and the collecting agent is kerosene; the weight ratio of the foaming agent is less than or equal to 300g/t of dry coal slime, and the weight ratio of the collecting agent is less than or equal to 1000g/t of dry coal slime; the aeration quantity of the primary purifying machine (8) is 0.6-1.2m 3 /(m 2 Min) and the rotating speed is 350r/min.
9. The process and apparatus for preparing nano-scale ultrapure carbon material from coal slime according to claim 1, wherein: the concentration of the primary purified ore pulp diluted by water in the S9 is 20-30g/l; the foaming agent in the S9 is sec-octanol, and the collecting agent is kerosene; the foaming agent is less than or equal to 200g/t of dry coal slime, and the collecting agent is less than or equal to 800g/t of dry coal slime; the aeration quantity of the secondary purifying machine (9) is 0.6-1.2m 3 /(m 2 Min) and the rotating speed is 350r/min.
10. The process and apparatus for preparing nano-scale ultrapure carbon material using coal slime as claimed in claim 1, wherein: the concentration of the secondary purified ore pulp diluted by water in the S10 is 15-20g/l; the foaming agent in the S10 is sec-octanol, and the collecting agent is kerosene; the foaming agent is less than or equal to 100g/t of dry coal slime, and the collecting agent is less than or equal to 500g/t of dry coal slime; the aeration quantity of the tertiary purifier (10) is 0.6-1.2m 3 /(m 2 Min), the rotating speed is 350r/min; the pressure of the filter press (11) in the S11 is7-10bar, and the ash content of the prepared nano-scale ultrapure carbon material is reduced to below 3 percent.
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