CN116355663A - Nanometer pulverized coal primary pulp, nanometer hydrocarbon fuel and preparation method thereof - Google Patents
Nanometer pulverized coal primary pulp, nanometer hydrocarbon fuel and preparation method thereof Download PDFInfo
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- 239000003245 coal Substances 0.000 title claims abstract description 168
- 239000000446 fuel Substances 0.000 title claims abstract description 45
- 239000004215 Carbon black (E152) Substances 0.000 title claims abstract description 40
- 229930195733 hydrocarbon Natural products 0.000 title claims abstract description 40
- 150000002430 hydrocarbons Chemical class 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 97
- 239000002245 particle Substances 0.000 claims abstract description 42
- 238000009826 distribution Methods 0.000 claims abstract description 19
- 238000007709 nanocrystallization Methods 0.000 claims abstract description 19
- 229910000831 Steel Inorganic materials 0.000 claims description 108
- 239000010959 steel Substances 0.000 claims description 108
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 62
- 229910052739 hydrogen Inorganic materials 0.000 claims description 60
- 239000001257 hydrogen Substances 0.000 claims description 60
- 239000002002 slurry Substances 0.000 claims description 59
- 238000000034 method Methods 0.000 claims description 46
- 238000010298 pulverizing process Methods 0.000 claims description 26
- 229920002873 Polyethylenimine Polymers 0.000 claims description 24
- 238000000227 grinding Methods 0.000 claims description 16
- 239000002270 dispersing agent Substances 0.000 claims description 15
- -1 1-tetradecyl-3-methylimidazole hexafluorophosphate Chemical compound 0.000 claims description 12
- PSZYNBSKGUBXEH-UHFFFAOYSA-M naphthalene-1-sulfonate Chemical compound C1=CC=C2C(S(=O)(=O)[O-])=CC=CC2=C1 PSZYNBSKGUBXEH-UHFFFAOYSA-M 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 9
- 239000002817 coal dust Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 5
- 238000005243 fluidization Methods 0.000 claims description 4
- 239000002105 nanoparticle Substances 0.000 claims description 2
- 238000000498 ball milling Methods 0.000 description 14
- 230000008569 process Effects 0.000 description 14
- 238000011049 filling Methods 0.000 description 12
- 239000000463 material Substances 0.000 description 12
- 230000001105 regulatory effect Effects 0.000 description 9
- 239000002994 raw material Substances 0.000 description 7
- 238000010998 test method Methods 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 230000002349 favourable effect Effects 0.000 description 5
- 238000004513 sizing Methods 0.000 description 5
- 238000002485 combustion reaction Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
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- 238000011161 development Methods 0.000 description 2
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- 239000000126 substance Substances 0.000 description 2
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000612182 Rexea solandri Species 0.000 description 1
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- 238000010420 art technique Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L1/00—Liquid carbonaceous fuels
- C10L1/32—Liquid carbonaceous fuels consisting of coal-oil suspensions or aqueous emulsions or oil emulsions
- C10L1/326—Coal-water suspensions
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
- C10L2290/28—Cutting, disintegrating, shredding or grinding
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
- C10L2290/56—Specific details of the apparatus for preparation or upgrading of a fuel
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crushing And Grinding (AREA)
Abstract
The invention provides nanometer pulverized coal primary pulp, nanometer hydrocarbon fuel and a preparation method thereof. The preparation method of the nanometer pulverized coal primary pulp comprises the following steps: primary crushing raw coal to obtain coarse coal powder, wherein the particle size distribution range D50 of the coarse coal powder is 325-800 meshes; less than 300 meshes of powder in the coarse coal powder is less than 8%, more than 40 meshes of powder is less than 5%, and more than 30 meshes of powder is 0; re-crushing the coarse coal powder by using an air jet mill to obtain fine coal powder, wherein the particle size distribution range D50 of the fine coal powder is 2-3 mu m; the fine coal powder is subjected to nanocrystallization and crushing by a wet ball mill, so as to obtain the nano coal powder primary pulp containing the nanocrystallized coal powder, wherein the particle size distribution range D50 of the nanocrystallized coal powder is 0.2-1.0 mu m. Can solve the problem that the nano pulverized coal is difficult to obtain in the prior art, and is suitable for the field of nano hydrocarbon fuel preparation.
Description
Technical Field
The invention relates to the field of nano hydrocarbon fuel preparation, in particular to nano pulverized coal primary pulp, nano hydrocarbon fuel and a preparation method thereof.
Background
The existing traditional coal has low combustion energy efficiency, low heat productivity and outstanding carbon emission problem, and a large amount of fly ash particles, sulfur dioxide, nitrogen compounds and other atmospheric pollutants can be generated in the combustion process. In recent years, along with the strong growth of energy consumption, particularly coal consumption in China, the clean and efficient development is more urgent, and the development of novel fuels with low cost and high fuel value becomes necessary.
The application of the coal water slurry has been developed in recent years, and the technical proposal for carrying out ultrafine grinding on coal has also appeared. However, the pulverizing method in the prior art is difficult to pulverize the pulverized coal to a nanocrystallization scale of 1 μm or less, and the pulverizing method in the prior art can cause a series of post-treatment procedures such as wastewater treatment, slurry drying and the like, and the pulverizing process is complex and the manufacturing cost is high.
Therefore, a preparation method of nano pulverized coal with simple process and low resource consumption is sought, which is very beneficial to the application field of coal and is also a key technical problem for preparing nano hydrocarbon fuel.
Disclosure of Invention
The invention mainly aims to provide nano pulverized coal primary pulp, nano hydrocarbon fuel and a preparation method thereof, so as to solve the problem that nano pulverized coal is difficult to obtain in the prior art.
In order to achieve the above object, according to a first aspect of the present invention, there is provided a method for preparing nano pulverized coal raw slurry, the method comprising: primary crushing raw coal to obtain coarse coal powder, wherein the particle size distribution range D50 of the coarse coal powder is 325-800 meshes; less than 300 meshes of powder in the coarse coal powder is less than 8%, more than 40 meshes of powder is less than 5%, and more than 30 meshes of powder is 0; re-crushing the coarse coal powder by using an air jet mill to obtain fine coal powder, wherein the particle size distribution range D50 of the fine coal powder is 2-3 mu m; the fine coal powder is subjected to nanocrystallization and crushing by a wet ball mill, so as to obtain the nano coal powder primary pulp containing the nanocrystallized coal powder, wherein the particle size distribution range D50 of the nanocrystallized coal powder is 0.2-1.0 mu m.
Further, the air flow mill comprises a negative pressure air flow mill; preferably, the parameters of the fine pulverization using the negative pressure jet mill include: the rotating speed of the classifying wheel is 8000-18000r/min, the grinding pressure is 0.7-0.8MPa, and the air consumption is 10-20m 3 Per min, nozzle velocity 1.25-1.95 mach, basic fluidization feed amount: 20-60 kg; preferably, the raw coal is subjected to primary crushing by a Raymond mill.
Further, the nanocrystallization includes: adding fine coal powder and water into a wet ball mill, mixing the fine coal powder and the water to form slurry, and carrying out nanocrystallization and crushing to obtain nano coal powder primary slurry.
Further, the mass content of the fine coal powder in the slurry is 35% -55%; the proportion of the total volume of the sizing agent and the steel ball to the total volume of the cavity of the wet ball mill is 40-80%; the mass ratio of the steel ball to the slurry is 2:1-1:1; the rotating speed of the wet ball mill is 15-80r/min; the grinding time of the wet ball mill is 1-6 hours;
further, the diameters of the steel balls include 20mm, 10mm, 8mm, 6mm, 4mm, 3mm, 2mm, 1mm and 0.5mm; preferably, the mass ratio of the 20mm steel ball is 5-15%; the mass ratio of the steel ball of 10mm is 5-8%; the mass ratio of the steel ball with the diameter of 8mm is 5-8%; the mass ratio of the steel ball of 6mm is 5-8%; the mass ratio of the steel ball with the diameter of 4mm is 5-8%; the mass ratio of the steel ball with the diameter of 3mm is 5-8%; the mass ratio of the steel ball with the diameter of 2mm is 10-15%; the mass ratio of the steel ball with the diameter of 1mm is 10-25%; the mass ratio of the steel ball with the thickness of 0.5mm is 10-25%.
Further, before nano-pulverizing, mixing fine coal powder, water and a dispersing agent to form slurry; preferably, the dispersant comprises naphthalene sulfonate polycondensate NSF, 1-tetradecyl-3-methylimidazole hexafluorophosphate and polyethylenimine L-PEI; preferably, the addition amount of naphthalene sulfonate polycondensate NSF is 1.6% -2.4%, the addition amount of 1-tetradecyl-3-methylimidazole hexafluorophosphate is 0.8-1.2% and the addition amount of polyethylenimine L-PEI is 0.2-0.5% based on the solid dry weight of nano hydrocarbon fuel.
In order to achieve the above object, according to a second aspect of the present invention, there is provided a method for producing nano hydrocarbon fuel, the method comprising: introducing hydrogen into the nano pulverized coal primary slurry prepared by the preparation method of the nano pulverized coal primary slurry to carry out hydrogen attaching energization treatment to obtain the nano hydrocarbon fuel.
Further, the hydrogen required by dry basis of each ton of nanometer pulverized coal primary pulp is 5.0-6.0m measured under room temperature and hydrogen pressure of 0.5-0.7MPa 3 The method comprises the steps of carrying out a first treatment on the surface of the Preferably, the concentration of hydrogen is > 90%.
Further, the hydrogen-attaching energizing treatment includes a microbubble method including: reducing the pressure of hydrogen to 0.05-0.2MPa, and then introducing the reduced pressure hydrogen into a micropore device arranged at the lowest end of the nano pulverized coal primary pulp, wherein the micropore gap of the micropore device is 0.5-20 mu m, so that the hydrogen passes through the nano pulverized coal primary pulp in a micro-bubble mode, and nano pulverized coal in the nano pulverized coal primary pulp adsorbs the hydrogen; preferably, the area above the nanometer pulverized coal primary pulp is subjected to negative pressure treatment, and overflowed hydrogen is emptied.
In order to achieve the above object, according to a third aspect of the present invention, there is provided a nano hydrocarbon fuel comprising the nano hydrocarbon fuel obtained by the above-described production method.
By adopting the technical scheme of the invention, raw coal is firstly subjected to coarse grinding to obtain coarse coal powder with a particle size suitable for a subsequent jet mill, and then the coarse coal powder is subjected to re-grinding by the jet mill to obtain fine coal powder. And then the wet ball mill is used for carrying out nanocrystallization on the fine coal powder to obtain the nano coal powder primary pulp containing the nanocrystallized coal powder. The method of graded crushing is utilized, the advantages of different crushing methods can be fully exerted, the graded crushing efficiency is higher, the process requirement on a single process is reduced, the production cost is convenient to control, and the production efficiency is improved.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention. In the drawings:
fig. 1 shows a schematic diagram of an apparatus for hydrogen addition enabling treatment in embodiment 1 according to the present invention.
Wherein the above figures include the following reference numerals:
1. a hydrogen gas input channel; 2. a microporous device; 3. hydrogen in the form of microbubbles; 4. a slurry; 5. a negative pressure device; 6. the hydrogen overflows the channel.
Detailed Description
It should be noted that, in the case of no conflict, the embodiments and features in the embodiments may be combined with each other. The present invention will be described in detail with reference to examples.
Term interpretation:
the nanocrystallized coal powder comprises coal particles with D50 less than or equal to 1 mu m.
As mentioned in the background art, it is difficult to pulverize coal into nano pulverized coal with D50 less than or equal to 1 μm. In the present application, the inventors tried to develop a method for preparing nano pulverized coal, and thus proposed a series of protection schemes of the present application.
In a first exemplary embodiment of the present application, there is provided a method for preparing nano pulverized coal raw slurry, the method comprising: primary crushing raw coal to obtain coarse coal powder, wherein the particle size distribution range D50 of the coarse coal powder is 325-800 meshes; less than 300 meshes of powder in the coarse coal powder is less than 8%, more than 40 meshes of powder is less than 5%, and more than 30 meshes of powder is 0; re-crushing the coarse coal powder by using an air jet mill to obtain fine coal powder, wherein the particle size distribution range D50 of the fine coal powder is 2-3 mu m; the fine coal powder is subjected to nanocrystallization and crushing by a wet ball mill, so as to obtain the nano coal powder primary pulp containing the nanocrystallized coal powder, wherein the particle size distribution range D50 of the nanocrystallized coal powder is 0.2-1.0 mu m.
In a preferred embodiment, the jet mill comprises a negative pressure jet mill; preferably, the parameters of the fine pulverization using the negative pressure jet mill include: the rotating speed of the classifying wheel is 8000-18000r/min, the grinding pressure is 0.7-0.8MPa, and the air consumption is 10-20m 3 Per min, nozzle velocity 1.25-1.95 mach, basic fluidization feed amount: 20-60 kg; preferably, the raw coal is initially crushed using prior art techniques including, but not limited to, raymond mills and the like.
In the preparation method of the nanometer pulverized coal primary slurry, raw material coal is coarsely crushed to obtain powder with proper particle size and no particle size of more than 30 meshes, and the powder is beneficial to being subsequently fed into an air flow mill for re-crushing. The three-time crushing of coarse crushing, re-crushing and nano crushing is convenient for controlling the particle size of the pulverized coal before each crushing, so that nano pulverized coal with more uniform particle size is obtained after nano crushing. Among the above parameters, the rotation speed of the classifying wheel affects the particle size of the finished product, the nozzle speed affects the crushing capacity, and the gas consumption affects the processing capacity per unit time. In the nanocrystallization crushing process, a plurality of parameters are needed to cooperate to act together, so that a good crushing effect can be realized.
For the nano-pulverization of the pulverized coal, if the air-jet mill method is adopted for the nano-pulverization of the "one-step", only a very small number of air-jet mills can achieve the pulverization result of 0.2-1 micron, and the equipment has strict direct pulverization process requirement, high cost, lower yield and lower economic benefit, and is not suitable for large-area popularization. In order to avoid the phenomenon, the invention adopts a common fluidized bed collision type jet mill (negative pressure) +a pulverizer combination of wet ball milling, and adopts a sectional type pulverizing method to carry out nanocrystallization pulverization, thereby finally achieving the same pulverizing effect. Compared with the one-step nano-crushing method, the fluidized bed collision type jet mill (negative pressure) control system in the combined nano-crushing method is simple, the total equipment price is lower, and the cost is lower. Because there is wet ball mill to pulverize for the second time, so the particle size requirement for fluid-bed collision type jet mill (negative pressure) pulverize is not very strict, pulverize in order to obtain finer particle in shorter time as the principle; the process requirements on the fluidized bed collision type jet mill (negative pressure) are not very strict, and the process is relatively easier to realize; the quality control is not required to be strict, and the cost is convenient to control.
In a preferred embodiment, the nanocrystallization includes: adding fine coal powder and water into a wet ball mill, mixing the fine coal powder and the water to form slurry, and carrying out nanocrystallization and crushing to obtain nano coal powder primary slurry.
In a preferred embodiment, the mass content of the fine coal powder in the slurry is 35% -55%; the proportion of the total volume of the sizing agent and the steel ball to the total volume of the cavity of the wet ball mill is 40-80%; the mass ratio of the steel ball to the slurry is 2:1-1:1; the rotating speed of the wet ball mill is 15-80r/min; the grinding time of the wet ball mill is 1-6 hours;
in a preferred embodiment, the diameter of the steel ball comprises 20mm, 10mm, 8mm, 6mm, 4mm, 3mm, 2mm, 1mm and 0.5mm; preferably, the mass ratio of the 20mm steel ball is 5-15%; the mass ratio of the steel ball of 10mm is 5-8%; the mass ratio of the steel ball with the diameter of 8mm is 5-8%; the mass ratio of the steel ball of 6mm is 5-8%; the mass ratio of the steel ball with the diameter of 4mm is 5-8%; the mass ratio of the steel ball with the diameter of 3mm is 5-8%; the mass ratio of the steel ball with the diameter of 2mm is 10-15%; the mass ratio of the steel ball with the diameter of 1mm is 10-25%; the mass ratio of the steel ball with the thickness of 0.5mm is 10-25%.
In the process of crushing the powder, the properties of different substances are completely different, so that the crushing conditions of different substances are also completely different, and the crushing conditions have no reference significance. In the application, the inventor finds that by using the parameters, the nano pulverized coal with the D50 of 0.2-1.0 μm which is difficult to obtain by a pulverizing method in the prior art with high efficiency or has high production cost can not only meet the pulverizing requirement, but also reduce the requirement on the production equipment process and the production cost.
In a preferred embodiment, the fine coal powder, water and dispersant are mixed to form a slurry prior to the nano-sized comminution; preferably, the dispersant comprises naphthalene sulfonate polycondensate NSF, 1-tetradecyl-3-methylimidazole hexafluorophosphate and polyethylenimine L-PEI; preferably, the addition amount of naphthalene sulfonate polycondensate NSF is 1.6% -2.4%, the addition amount of 1-tetradecyl-3-methylimidazole hexafluorophosphate is 0.8-1.2% and the addition amount of polyethylenimine L-PEI is 0.2-0.5% based on the solid dry weight of nano hydrocarbon fuel.
In the nanocrystallization crushing process, because the coal dust has serious hydrophobicity, in order to uniformly disperse the coal dust into water, agglomeration among particles is reduced, and better fluidity of slurry is achieved, so that a dispersing agent is added in the nanocrystallization crushing process, the dispersing agent mainly has the effects of increasing the fluidity of slurry, promoting the dispersion of the coal dust in the water and facilitating the nanocrystallization crushing. Meanwhile, the resistance among the pulverized coal is reduced, the viscosity is reduced, the agglomeration phenomenon of nanoscale material particles is solved, and the stability of the prepared nano pulverized coal primary slurry in the neutral state in the storage and transportation processes is ensured.
In a second exemplary embodiment of the present application, there is provided a method for preparing nano hydrocarbon fuel, the method comprising: introducing hydrogen into the nano pulverized coal primary slurry prepared by the preparation method for hydrogen attaching energizing treatment to obtain the nano hydrocarbon fuel.
In a preferred embodiment, the hydrogen required per ton of dry basis of the nano-pulverized coal primary slurry is 5.0-6.0m measured at room temperature under a hydrogen pressure of 0.5-0.7MPa 3 The method comprises the steps of carrying out a first treatment on the surface of the Preferably, the concentration of hydrogen is > 90%. The above room temperature conditions include 15-30deg.C.
In a preferred embodiment, the hydrogen-attaching energizing treatment comprises a microbubble process comprising: reducing the pressure of hydrogen to 0.05-0.2MPa, and then introducing the reduced pressure hydrogen into a micropore device arranged at the lowest end of the nano pulverized coal primary pulp, wherein the micropore gap of the micropore device is 0.5-20 mu m, so that the hydrogen passes through the nano pulverized coal primary pulp in a micro-bubble mode, and nano pulverized coal in the nano pulverized coal primary pulp adsorbs the hydrogen; preferably, the area above the nanometer pulverized coal primary pulp is subjected to negative pressure treatment, and overflowed hydrogen is emptied.
The hydrogen is introduced into the nanometer pulverized coal primary pulp, and because the pulverized coal in the nanometer pulverized coal primary pulp is micro-nanometer superfine powder, the specific surface area and the surface energy are larger, and the introduced hydrogen can be adsorbed on superfine powder particles, thereby achieving the purpose of hydrogen attachment. The negative pressure device is arranged on the upper part of the nano pulverized coal primary pulp, the negative pressure treatment is carried out on the area above the nano pulverized coal primary pulp, overflowed hydrogen can be emptied, the emptied hydrogen can be explosion-proof, and the hydrogen can be recycled.
In a third exemplary embodiment of the present application, there is provided a nano hydrocarbon fuel including the nano hydrocarbon fuel prepared by the above-described preparation method.
The advantageous effects of the present application will be explained in further detail below in connection with specific examples.
Example 1
1. Primary crushing of raw coal
The raw material coal used in the embodiment is refined coal in an inner Mongolian quaiger mining area, the raw material coal is subjected to primary crushing by a Raymond mill, dry crushing is adopted, and the particle size distribution D50 of the pulverized coal after primary crushing is 500 meshes; powder smaller than 300 meshes is smaller than 8%; powder with the particle size of more than 40 meshes is less than 5 percent; powder with the particle size of more than 30 meshes is 0.
2. Re-crushing
And (3) re-crushing the coarse coal powder after primary crushing by using a fluidized bed collision type jet mill (negative pressure). Fine coal dust with a particle diameter D50 of 2.4 μm was obtained.
The parameters of the fluidized bed collision type jet mill (negative pressure) are as follows: the rotating speed of the classifying wheel is 10000r/min; grinding pressure is 0.75MPa; air consumption 13m 3 A/min; nozzle speed mach 1.35; basic fluidization state feed amount: 30 kg.
3. Nanocrystallization crushing
In this example, a wet ball mill was used to nano-pulverize the fine coal powder. The particle size distribution D50 of the nano pulverized coal particles in the nano pulverized coal primary slurry obtained by crushing is 0.8 micron. Specific parameters of wet ball milling:
filling ratio: namely the volume of the materials and the steel balls and the total volume of the cavity of the ball mill are in proportion, and the filling ratio of the wet ball mill in the embodiment is 70 percent.
Ball-to-material ratio: i.e. the mass ratio of the steel ball to the slurry is 3:2.
Slurry concentration: 50%.
Adding a dispersant when mixing to obtain a slurry, the dispersant comprising:
A. naphthalene sulfonate polycondensate (NSF);
B. 1-tetradecyl-3-methylimidazole hexafluorophosphate ([ C) 14 MIm][PF 6 ])；
C. Polyethylenimine (L-PEI).
The addition amount of the dispersing agent is as follows:
the addition amount is 2.0 percent of the addition amount of the A, naphthalene sulfonate polycondensate (NSF) based on the dry weight of nano hydrocarbon fuel solid; B. 1-tetradecyl-3-methylimidazole hexafluorophosphate ([ C) 14 MIm][PF 6 ]) The addition amount is 0.9 per mill; C. the addition amount of polyethylenimine (L-PEI) is 0.35 per mill.
The ratio of the balls is as follows: the diameters of steel balls in the wet ball mill are respectively 20mm, 10mm, 8mm, 6mm, 4mm, 3mm, 2mm, 1mm and 0.5mm, and the matching is carried out according to the following proportion: the mass ratio of the steel ball with the diameter of 20mm is 10%; the mass ratio of the steel ball of 10mm is 7%; the mass ratio of the steel ball with the diameter of 8mm is 7%; the mass ratio of the steel ball of 6mm is 7%; the mass ratio of the steel ball with the diameter of 4mm is 7%; the mass ratio of the steel ball with the diameter of 3mm is 7%; the mass ratio of the steel ball with the diameter of 2mm is 13%; the mass ratio of the steel ball of 1mm is 21%; the mass ratio of the steel ball of 0.5mm is 21%;
ball milling rotating speed: 45r/min.
Grinding duration: 2.5 hours.
The yield of the nano coal dust primary pulp for 2.5 hours is 400 kg.
4. Hydrogen-attached energizing treatment
Taking nano coal dust primary pulp with slurry concentration of 50% of 1 ton as an example, hydrogen attaching parameters:
1) The concentration of the introduced hydrogen was 95%;
2) The hydrogen required to be introduced is 2.8m 3 ；
3) The initial pressure of the introduced hydrogen is 0.6MPa, and the pressure is reduced to 0.012MPA after the pressure is regulated by a pressure regulating device;
4) The introduction mode is a micro-bubble method, hydrogen after being depressurized by a pressure regulating device is introduced into the bottommost part of slurry from a hydrogen input channel 1, and is introduced into a micro-pore device 2, the micro-pore gap of the micro-pore device 2 is 2 microns, so that the hydrogen passes through the slurry 4 in a micro-bubble mode through the hydrogen 3, meanwhile, a negative pressure device 5 is arranged at the upper part of the slurry 4, overflowed hydrogen is emptied from a hydrogen overflow channel 6, the purpose of emptying is explosion-proof, and the hydrogen can be recycled. The apparatus for the hydrogen-attaching energizing process includes, but is not limited to, the apparatus shown in fig. 1. Preparing and obtaining the nano hydrocarbon fuel.
The apparent viscosity test method comprises the following steps: the shear rate was 100s using a German Hake VT550 type rotational viscometer -1 Average of 10 data recorded.
The burn-up rate test method comprises the following steps: drying the upper coal-based fuel, weighing, and recording the weight of the dry coal-based fuel as M 1 Fully burning coal-based fuel at 850 ℃, collecting silicon-aluminum powder obtained after combustion, weighing and marking as M 2 Burnout rate= (M 1 -M 2 )/M 1 。
The apparent viscosity data of the nano hydrocarbon fuel prepared in this example are shown in table 1. The burnout rate and the heat value data of the nano hydrocarbon fuel prepared in this example are shown in table 2.
Example 2
The preparation method adopted in this example is the same as that adopted in example 1, and is favorable for nano-pulverizing the fine coal powder obtained in the preparation in example 1, and the particle size distribution D50 of nano-pulverized coal particles in the nano-pulverized coal primary slurry obtained by pulverizing is 0.95 μm, except that specific parameters of a wet ball mill are different.
Specific parameters of wet ball milling:
filling ratio: namely the volume of the materials and the steel balls and the total volume of the cavity of the ball mill are in proportion, and the filling ratio of wet ball milling in the embodiment is 40%.
Ball-to-material ratio: i.e. the mass ratio of the steel ball to the slurry is 3:2.
Slurry concentration: 55%.
The ratio of the balls is as follows: the diameters of steel balls in the wet ball mill are respectively 20mm, 10mm, 8mm, 6mm, 4mm, 3mm, 2mm, 1mm and 0.5mm, and the matching is carried out according to the following proportion: the mass ratio of the steel ball with the diameter of 20mm is 15%; the mass ratio of the steel ball of 10mm is 8%; the mass ratio of the steel ball with the diameter of 8mm is 8%; the mass ratio of the steel ball of 6mm is 8%; the mass ratio of the steel ball with the diameter of 4mm is 8%; the mass ratio of the steel ball with the diameter of 3mm is 8%; the mass ratio of the steel ball with the diameter of 2mm is 15%; the mass ratio of the steel ball of 1mm is 20%; the mass ratio of the steel ball of 0.5mm is 10%;
ball milling rotating speed: 15r/min.
Grinding duration: 2.5 hours.
The yield of the nanometer pulverized coal primary pulp for 2.5 hours is 300 kg.
Example 3
The preparation method adopted in this example is the same as that adopted in example 1, and is favorable for nano-pulverizing the fine coal powder obtained in the preparation in example 1, and the particle size distribution D50 of nano-pulverized coal particles in the nano-pulverized coal primary slurry obtained by pulverizing is 0.2 μm, except that specific parameters of a wet ball mill are different.
Specific parameters of wet ball milling:
filling ratio: namely the volume of the materials and the steel balls and the total volume of the cavity of the ball mill, and the filling ratio of the wet ball mill in the embodiment is 80 percent.
Ball-to-material ratio: i.e. the mass ratio of the steel ball to the sizing agent is 2:1.
Slurry concentration: 35%.
The ratio of the balls is as follows: the diameters of steel balls in the wet ball mill are respectively 20mm, 10mm, 8mm, 6mm, 4mm, 3mm, 2mm, 1mm and 0.5mm, and the matching is carried out according to the following proportion: the mass ratio of the steel ball with the diameter of 20mm is 10%; the mass ratio of the steel ball of 10mm is 5%; the mass ratio of the steel ball with the diameter of 8mm is 5%; the mass ratio of the steel ball of 6mm is 5%; the mass ratio of the steel ball with the diameter of 4mm is 5%; the mass ratio of the steel ball with the diameter of 3mm is 5%; the mass ratio of the steel ball with the diameter of 2mm is 15%; the mass ratio of the steel ball of 1mm is 25%; the mass ratio of the steel ball of 0.5mm is 25%;
ball milling rotating speed: 80r/min.
Grinding duration: 2.5 hours.
The yield of the nanometer pulverized coal primary pulp for 2.5 hours is 300 kg.
Example 4
The preparation method adopted in this example is the same as that adopted in example 1, and is favorable for nano-pulverizing the fine coal powder obtained in the preparation in example 1, and the particle size distribution D50 of nano-pulverized coal particles in the nano-pulverized coal primary slurry obtained by pulverizing is 0.8 μm, except that specific parameters of a wet ball mill are different.
Specific parameters of wet ball milling:
filling ratio: namely the volume of the materials and the steel balls and the total volume of the cavity of the ball mill are in proportion, and the filling ratio of the wet ball mill in the embodiment is 70 percent.
Ball-to-material ratio: i.e. the mass ratio of the steel ball to the sizing agent is 1:1.
Slurry concentration: 50%.
The ratio of the balls is as follows: the diameters of steel balls in the wet ball mill are respectively 20mm, 10mm, 8mm, 6mm, 4mm, 3mm, 2mm, 1mm and 0.5mm, and the matching is carried out according to the following proportion: the mass ratio of the steel ball of 20mm is 5%; the mass ratio of the steel ball of 10mm is 7%; the mass ratio of the steel ball with the diameter of 8mm is 7%; the mass ratio of the steel ball of 6mm is 7%; the mass ratio of the steel ball with the diameter of 4mm is 7%; the mass ratio of the steel ball with the diameter of 3mm is 7%; the mass ratio of the steel ball of 2mm is 14%; the mass ratio of the steel ball of 1mm is 23%; the mass ratio of the steel ball of 0.5mm is 23%;
ball milling rotating speed: 45r/min.
Grinding duration: 2.5 hours.
The yield of the nanometer pulverized coal primary pulp for 2.5 hours is 350 kg.
Example 5
The preparation method adopted in this example is the same as that adopted in example 1, and is favorable for nano-pulverizing the fine coal powder obtained in the preparation in example 1, and the particle size distribution D50 of nano-pulverized coal particles in the nano-pulverized coal primary slurry obtained by pulverizing is 0.8 μm, except that specific parameters of a wet ball mill are different.
Specific parameters of wet ball milling:
filling ratio: namely the volume of the materials and the steel balls and the total volume of the cavity of the ball mill are in proportion, and the filling ratio of the wet ball mill in the embodiment is 70 percent.
Ball-to-material ratio: i.e. the mass ratio of the steel ball to the slurry is 1:3.
Slurry concentration: 50%.
The ratio of the balls is as follows: the diameters of steel balls in the wet ball mill are respectively 20mm, 10mm, 8mm, 6mm, 4mm, 3mm, 2mm, 1mm and 0.5mm, and the matching is carried out according to the following proportion: the mass ratio of the steel ball of 20mm is 5%; the mass ratio of the steel ball of 10mm is 7%; the mass ratio of the steel ball with the diameter of 8mm is 7%; the mass ratio of the steel ball of 6mm is 7%; the mass ratio of the steel ball with the diameter of 4mm is 7%; the mass ratio of the steel ball with the diameter of 3mm is 7%; the mass ratio of the steel ball of 2mm is 14%; the mass ratio of the steel ball of 1mm is 23%; the mass ratio of the steel ball of 0.5mm is 23%;
ball milling rotating speed: 45r/min.
Grinding duration: 8 hours.
The yield of the nanometer pulverized coal primary pulp for 8 hours is 280 kg.
Example 6
The preparation method adopted in this example is the same as that adopted in example 1, and is favorable for nano-pulverizing the fine coal powder obtained in the preparation in example 1, and the particle size distribution D50 of nano-pulverized coal particles in the nano-pulverized coal primary slurry obtained by pulverizing is 0.8 μm, except that specific parameters of a wet ball mill are different.
Specific parameters of wet ball milling:
filling ratio: namely the volume of the materials and the steel balls and the total volume of the cavity of the ball mill are in proportion, and the filling ratio of the wet ball mill in the embodiment is 30 percent.
Ball-to-material ratio: i.e. the mass ratio of the steel ball to the sizing agent is 1:1.
Slurry concentration: 50%.
The ratio of the balls is as follows: the diameters of steel balls in the wet ball mill are respectively 20mm, 10mm, 8mm, 6mm, 4mm, 3mm, 2mm, 1mm and 0.5mm, and the matching is carried out according to the following proportion: the mass ratio of the steel ball with the diameter of 20mm is 15%; the mass ratio of the steel ball of 10mm is 15%; the mass ratio of the steel ball with the diameter of 8mm is 15%; the mass ratio of the steel ball of 6mm is 15%; the mass ratio of the steel ball with the diameter of 4mm is 10%; the mass ratio of the steel ball with the diameter of 3mm is 6%; the mass ratio of the steel ball of 2mm is 8%; the mass ratio of the steel ball of 1mm is 8%; the mass ratio of the steel ball of 0.5mm is 8%;
ball milling rotating speed: 45r/min.
Grinding duration: and 12 hours.
The yield of the nano coal dust primary pulp for 12 hours is 280 kg.
Example 7
The nano hydrocarbon fuel was prepared using the raw materials and the method of example 1, differing from example 1 in that the dispersant used in this example includes:
the addition amount is 1.6 percent of the addition amount of the A, naphthalene sulfonate polycondensate (NSF) based on the dry weight of nano hydrocarbon fuel solid; B. 1-tetradecyl-3-methylimidazole hexafluorophosphate ([ C) 14 MIm][PF 6 ]) The addition amount is 1.2 per mill; C. the addition amount of polyethylenimine (L-PEI) is 0.5 per mill.
The apparent viscosity test method of this example is the same as that of example 1, and specific data are shown in table 1.
Example 8
The nano hydrocarbon fuel was prepared using the raw materials and the method of example 1, differing from example 1 in that the dispersant used in this example includes:
the addition amount is 2.4 percent of the addition amount of the A, naphthalene sulfonate polycondensate (NSF) based on the dry weight of nano hydrocarbon fuel solid; B. 1-tetradecyl-3-methylimidazole hexafluorophosphate ([ C) 14 MIm][PF 6 ]) The addition amount is 0.8 per mill; C. the addition amount of polyethylenimine (L-PEI) is 0.2 per mill.
The apparent viscosity test method of this example is the same as that of example 1, and specific data are shown in table 1.
Example 9
The nano hydrocarbon fuel was prepared using the raw materials and the method of example 1, differing from example 1 in that the dispersant used in this example includes:
the addition amount is 1.5 percent of the addition amount of the A, naphthalene sulfonate polycondensate (NSF) based on the dry weight of nano hydrocarbon fuel solids; B. 1-tetradecyl-3-methylimidazole hexafluorophosphate ([ C) 14 MIm][PF 6 ]) The addition amount is 2 per mill; C. the addition amount of polyethyleneimine (L-PEI) is 1 per mill.
The apparent viscosity test method of this example is the same as that of example 1, and specific data are shown in table 1.
Example 10
The nano hydrocarbon fuel was prepared using the raw materials and the method of example 1, differing from example 1 in that the dispersant used in this example includes:
the addition amount is 2.5 percent of the addition amount of the A, naphthalene sulfonate polycondensate (NSF) based on the dry weight of nano hydrocarbon fuel solid; B. 1-tetradecyl-3-methylimidazole hexafluorophosphate ([ C) 14 MIm][PF 6 ]) The addition amount is 0.6 per mill; C. the addition amount of polyethylenimine (L-PEI) is 0.1 per mill.
The apparent viscosity test method of this example is the same as that of example 1, and specific data are shown in table 1.
TABLE 1
| Apparent viscosity (mPa.s) | |
| Example 1 | 500 |
| Example 7 | 507 |
| Example 8 | 495 |
| Example 9 | 588 |
| Example 10 | 438 |
The D50 is between 480 and 550mPa.s of excellent apparent viscosity of the nano hydrocarbon fuel with the diameter of 0.2 to 1.0 mu m.
Example 11
The nano raw slurry prepared in example 1 is used to prepare nano hydrocarbon fuel, which is different from example 1 in that the hydrogen attaching parameters in this example are:
1) The concentration of the introduced hydrogen was 85%;
2) The hydrogen required to be introduced is 2.1m 3 ；
3) The initial pressure of the introduced hydrogen is 0.6MPa, and the pressure is reduced to 0.012MPa after the pressure is regulated by a pressure regulating device;
4) The introduction mode is a micro-bubble method, hydrogen after being depressurized by a pressure regulating device is introduced to the bottommost part of the slurry, and the micropore gap of a micropore device is 2 microns.
Example 12
The nano raw slurry prepared in example 1 is used to prepare nano hydrocarbon fuel, which is different from example 1 in that the hydrogen attaching parameters in this example are:
1) The concentration of the introduced hydrogen was 95%;
2) The hydrogen required to be introduced is 3.5m 3 ；
3) The initial pressure of the introduced hydrogen is 0.8MPa, and the pressure is reduced to 0.012MPa after the pressure is regulated by a pressure regulating device;
4) The introduction mode is a micro-bubble method, hydrogen after being depressurized by a pressure regulating device is introduced to the bottommost part of the slurry, and the micropore gap of a micropore device is 2 microns.
The test method of burnout rate and heat value of this example was the same as that of example 1, and specific data are shown in table 2.
TABLE 2
| Solid calorific value (Daka/kg) | Burn-out rate (%) | |
| Example 1 | 4065 | 98.58 |
| Example 11 | 3985 | 98.36 |
| Example 12 | 3990 | 98.37 |
From the above description, it can be seen that the above embodiments of the present invention achieve the following technical effects: in the invention, raw coal is firstly subjected to primary crushing to obtain coarse coal powder with smaller particle size, and then the coarse coal powder is subjected to nanocrystallization crushing by using an air current mill, so that fine coal powder with D50 of 2-3 mu m can be obtained. Then the fine coal powder is subjected to nanocrystallization and crushing in a wet ball mill, so that the nano coal powder primary pulp with target concentration can be directly obtained, the nano coal powder primary pulp contains the nanocrystallized coal powder with D50 of 0.2-1.0 mu m, and the problem that the nanocrystallized coal powder is difficult to obtain in the prior art is solved. And introducing hydrogen into the nano pulverized coal primary slurry, wherein the nano pulverized coal with large specific surface area can adsorb the hydrogen, so that hydrogen-attached energization is realized, and the nano hydrocarbon fuel with better heat value and better performance is prepared.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. 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 method for preparing nano pulverized coal primary pulp, which comprises the following steps:
primary crushing raw coal to obtain coarse coal powder, wherein the particle size distribution range D50 of the coarse coal powder is 325-800 meshes; powder with less than 300 meshes in the coarse coal powder is less than 8%, powder with more than 40 meshes is less than 5%, and powder with more than 30 meshes is 0;
re-crushing the coarse coal powder by using an air flow mill to obtain fine coal powder, wherein the particle size distribution range D50 of the fine coal powder is 2-3 mu m;
and carrying out nanocrystallization crushing on the fine coal powder by utilizing a wet ball mill to obtain nano coal powder primary pulp containing nanocrystallized coal powder, wherein the particle size distribution range D50 of the nanocrystallized coal powder is 0.2-1.0 mu m.
2. The method of manufacturing according to claim 1, wherein the air-jet mill comprises a negative pressure air-jet mill;
preferably, the parameters of the fine pulverization using the negative pressure jet mill include:
the rotating speed of the classifying wheel is 8000-18000r/min, the grinding pressure is 0.7-0.8MPa, and the air consumption is 10-20m 3 Per min, nozzle velocity 1.25-1.95 mach, basic fluidization feed amount: 20-60 kg;
preferably, the primary crushing is performed on the raw coal using a raymond mill.
3. The method of claim 1, wherein the nanocrystallizing comprises: adding the fine coal powder and water into the wet ball mill, mixing the fine coal powder and the water to form slurry, and carrying out nanocrystallization and crushing to obtain the nano coal powder primary slurry.
4. A method of producing according to claim 3, wherein the mass content of the fine coal in the slurry is 35% to 55%;
the ratio of the total volume of the slurry and the steel balls to the total volume of the cavity of the wet ball mill is 40-80%;
the mass ratio of the steel ball to the slurry is 2:1-1:1;
the rotating speed of the wet ball mill is 15-80r/min;
the grinding duration of the wet ball mill is 1-6 hours.
5. The method of claim 4, wherein the diameter of the steel ball comprises 20mm, 10mm, 8mm, 6mm, 4mm, 3mm, 2mm, 1mm, and 0.5mm;
preferably, the mass ratio of the 20mm steel ball is 5-15%; the mass ratio of the steel ball of 10mm is 5-8%; the mass ratio of the steel ball with the diameter of 8mm is 5-8%; the mass ratio of the steel ball of 6mm is 5-8%; the mass ratio of the steel ball with the diameter of 4mm is 5-8%; the mass ratio of the steel ball with the diameter of 3mm is 5-8%; the mass ratio of the steel ball with the diameter of 2mm is 10-15%; the mass ratio of the steel ball with the diameter of 1mm is 10-25%; the mass ratio of the steel ball with the thickness of 0.5mm is 10-25%.
6. The method of claim 3, wherein the fine coal powder, the water and the dispersant are mixed to form the slurry prior to the nano-sized comminution;
preferably, the dispersant comprises naphthalene sulfonate polycondensate NSF, 1-tetradecyl-3-methylimidazole hexafluorophosphate and polyethylenimine L-PEI;
preferably, based on the solid dry weight of the nano hydrocarbon fuel, the addition amount of the naphthalene sulfonate polycondensate NSF is 1.6% -2.4%, the addition amount of the 1-tetradecyl-3-methylimidazole hexafluorophosphate is 0.8-1.2 per mill, and the addition amount of the polyethyleneimine L-PEI is 0.2-0.5 per mill.
7. A method for preparing nano hydrocarbon fuel, which is characterized by comprising the following steps:
introducing hydrogen into the nano coal dust raw slurry prepared by the preparation method of any one of claims 1 to 6 for hydrogen attaching energization treatment to obtain the nano hydrocarbon fuel.
8. The method according to claim 7, wherein the hydrogen gas required per ton of dry basis of the nano pulverized coal primary slurry is 5.0-6.0m measured under room temperature conditions and hydrogen gas pressure of 0.5-0.7MPa 3 ；
Preferably, the concentration of hydrogen is > 90%.
9. The production method according to claim 7 or 8, wherein the hydrogen attaching energizing treatment comprises a microbubble method comprising:
reducing the pressure of the hydrogen to 0.05-0.2MPa, and then introducing the reduced pressure hydrogen into a micropore device arranged at the lowest end of the nano pulverized coal primary slurry, wherein the micropore gap of the micropore device is 0.5-20 mu m, so that the hydrogen passes through the nano pulverized coal primary slurry in a micro-bubble mode, and the nano pulverized coal in the nano pulverized coal primary slurry adsorbs the hydrogen;
preferably, the region above the nanometer pulverized coal primary pulp is subjected to negative pressure treatment, and the overflowed hydrogen is emptied.
10. A nano hydrocarbon fuel, characterized in that the nano hydrocarbon fuel comprises a nano hydrocarbon fuel obtained by the production method according to any one of claims 7 to 9.
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