CN118620640A - Method for preparing precursor of coal bonding component - Google Patents
Method for preparing precursor of coal bonding component Download PDFInfo
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- CN118620640A CN118620640A CN202410642172.2A CN202410642172A CN118620640A CN 118620640 A CN118620640 A CN 118620640A CN 202410642172 A CN202410642172 A CN 202410642172A CN 118620640 A CN118620640 A CN 118620640A
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- toluene
- molecular sieve
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- 239000003245 coal Substances 0.000 title claims abstract description 104
- 239000002243 precursor Substances 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 19
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 99
- 239000002808 molecular sieve Substances 0.000 claims abstract description 29
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000000284 extract Substances 0.000 claims abstract description 27
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002608 ionic liquid Substances 0.000 claims abstract description 19
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000005804 alkylation reaction Methods 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims description 18
- 230000029936 alkylation Effects 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 238000002390 rotary evaporation Methods 0.000 claims description 9
- 239000000047 product Substances 0.000 claims description 8
- 230000002152 alkylating effect Effects 0.000 claims description 6
- RHZUVFJBSILHOK-UHFFFAOYSA-N anthracen-1-ylmethanolate Chemical compound C1=CC=C2C=C3C(C[O-])=CC=CC3=CC2=C1 RHZUVFJBSILHOK-UHFFFAOYSA-N 0.000 claims description 6
- 239000003830 anthracite Substances 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 239000007795 chemical reaction product Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- IPILPUZVTYHGIL-UHFFFAOYSA-M tributyl(methyl)azanium;chloride Chemical compound [Cl-].CCCC[N+](C)(CCCC)CCCC IPILPUZVTYHGIL-UHFFFAOYSA-M 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 230000010355 oscillation Effects 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 238000010025 steaming Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 abstract description 10
- 238000004939 coking Methods 0.000 abstract description 9
- 239000000571 coke Substances 0.000 abstract description 6
- 238000000605 extraction Methods 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 3
- 238000002844 melting Methods 0.000 abstract description 2
- 239000002168 alkylating agent Substances 0.000 abstract 1
- 229940100198 alkylating agent Drugs 0.000 abstract 1
- 230000003197 catalytic effect Effects 0.000 abstract 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 abstract 1
- 125000003118 aryl group Chemical group 0.000 description 3
- 150000001491 aromatic compounds Chemical class 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
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- Solid Fuels And Fuel-Associated Substances (AREA)
Abstract
The invention discloses a method for preparing a precursor of a coal bonding component, and relates to the technical field of comprehensive utilization of coal. According to the method, toluene hot-melting treatment is carried out on the long flame coal by using ionic liquid, based on the damage of the ionic liquid to the molecular structure of the long flame coal, polycyclic aromatic hydrocarbon in the long flame coal is enabled to be free in toluene solution, aromatic hydrocarbon is obtained through extraction of hot solution, then n-heptane and n-butanol are used as alkylating agents, beta molecular sieve is used as a catalyst, alkylation reaction is carried out through catalytic extraction of aromatic hydrocarbon, and the branching degree is increased. The results show that the alkylated extract can significantly improve the cohesiveness of the non-caking long flame coal. The study of the structure and composition of the alkylated extract can be used to reveal the molecular structure and composition of the precursor of the coal binding component. The invention realizes the preparation of the precursor of the coal bonding component by utilizing the extraction and alkylation reaction of the ionic liquid, can promote the knowledge of the molecular structure of the coal bonding component, and can provide theoretical guidance for improving the quality of coke and saving coking coal sources.
Description
Technical Field
The invention belongs to the technical field of comprehensive utilization of coal, and particularly relates to a method for preparing a precursor of a coal bonding component.
Background
The steel industry is the mainstay industry of national economy. So far, the role of coke in a material column skeleton in blast furnace ironmaking is not replaced. Coking coal is an essential raw material for preparing coke, but the coking coal has strong cohesiveness in China and less high-quality coking coal reserves which can be used for refining metallurgical coke. The low-rank coal reserves in China are rich and account for about 55% of the ascertained coal reserves in China. However, the caking property of low-rank coal is poor, and the blending amount of the low-rank coal directly used for blending coal coking is generally not more than 3%. In order to increase the amount of low-rank coal blended for coking, it is necessary to increase the cohesiveness. The coal degree of the low-rank coal is low, the macromolecular framework of the low-rank coal is mainly composed of aromatic compounds with 1-2 rings, and the aromatic compounds are connected with each other through different bridging bonds (such as alkyl bonds, ether bonds and the like) to form a complex network structure. Meanwhile, in the gaps of these macromolecular skeletons, there are also some low molecular compounds such as aliphatic hydrocarbons, aromatic hydrocarbons, oxygen-containing compounds, and the like. The poor caking properties of low rank coals are mainly due to their low content of caking components. At present, research on molecular structures of coal bonding components is still in an exploration stage, and consensus is not reached yet. Qualitative description of molecular structure of the coal-binding component it is stated that aromatic hydrocarbons of the appropriate number of rings with the appropriate alkyl chains are important precursors of the coal-binding component.
The ionic liquid exists in the form of liquid salt at room temperature or slightly above room temperature, and has better dissolving capacity. Under mild conditions, the ionic liquid can break chemical bonds or non-chemical bonds in the coal, and molecular fragments containing aromatic hydrocarbon are cut out. The aromatic hydrocarbon structure in the long flame coal is loose, the number of rings is less, the cross-linking structure is simple, and the cross-linking structure is easy to damage, so that the long flame coal can be treated by using an ionic liquid organic solvent for heat-melting to obtain aromatic hydrocarbon. Beta molecular sieves are a very important catalyst that exhibits excellent performance in catalyzing alkylation reactions, and thus beta molecular sieves are used as catalysts for extracting aromatic alkylation. In summary, the ionic liquid organic solvent is utilized to thermally dissolve the long flame coal to extract aromatic hydrocarbon, the beta molecular sieve is utilized to catalyze the alkylation of the aromatic hydrocarbon, and the branching degree of the extracted aromatic hydrocarbon is improved, so that the precursor of the coal bonding component is prepared, the precursor is used for improving the bonding property of low-rank coal, the understanding of the molecular structure of the coal bonding component can be promoted, and theoretical guidance is provided for saving coking coal sources.
Disclosure of Invention
The invention aims to provide a method for preparing a coal bonding component precursor, which utilizes ionic liquid extraction and alkylation reaction to prepare the coal bonding component precursor, realizes the purpose of preparing the coal bonding component precursor for improving the cohesiveness of long flame coal, can promote the understanding of the molecular structure of the coal bonding component, and can further provide theoretical guidance for improving the quality of coke and saving coking coal sources.
The aim of the invention can be achieved by the following technical scheme:
a method of preparing a precursor of a coal cementitious component comprising the steps of:
1) Respectively crushing and sieving air-dried long flame coal and fat coal to obtain granular samples, and sealing and preserving for later use;
2) Uniformly mixing 5g of long flame coal obtained in the step 1), 3g of tributyl methyl ammonium chloride ionic liquid and 20ml of toluene solution, heating at a certain temperature for a certain time, and cooling to room temperature to obtain a sample I;
3) Transferring the sample prepared in the step 2) into a centrifuge tube, centrifuging for 4min at a speed of 8000r/min, collecting upper liquid, adding fresh toluene (20 ml) into residual coal, performing ultrasonic oscillation for 5min, continuing centrifugal separation according to the centrifugal speed, cleaning for several times by the method until the upper liquid is nearly colorless, and recording filtrate as a sample II;
4) Carrying out reduced pressure rotary evaporation treatment on the second sample obtained in the step 3) at 55 ℃ for 20min to remove toluene, then adding absolute ethyl alcohol, carrying out reduced pressure rotary evaporation twice to sufficiently remove toluene, then adding distilled water, transferring a suspension formed by the extract, the ionic liquid and the distilled water into a centrifuge tube, centrifuging for 4min at a speed of 8000r/min, collecting a lower solid, and vacuum drying the lower solid to obtain the extract, and marking the extract as a third sample; the collected upper liquid can be recycled after rotary evaporation, and the ionic liquid can be reused;
5) Adding the sample III into a hydrothermal kettle, adding 5g of toluene as a solvent, 10g of n-heptane and 5g of n-butanol as an alkylating solvent, adding 0.3g of activated beta molecular sieve, and reacting for 4 hours at a set temperature; and centrifugally collecting reaction products, washing the molecular sieve until the molecular sieve is transparent by using toluene, and rotationally steaming centrifugate to remove toluene and an alkylation solvent to obtain the product.
Further, the reaction parameters of step 2) are: heating in a hydrothermal kettle at 70-160deg.C for 6-24 hr.
Further, the alkylation temperature in step 5) is 150-190 ℃.
Further, the beta molecular sieve in step 5) is activated by: and placing the beta molecular sieve in a cupel, and calcining for 2 hours in an air atmosphere at 550 ℃ by using a muffle furnace to remove the template agent, so as to obtain the activated beta molecular sieve.
Further, in order to verify the adhesive properties of the product, the effect of the product on the adhesion of the raw long flame coal was determined as follows:
Because the raw flame coal has no caking property, mixing the raw flame coal, fat coal and standard anthracite at a mass ratio of 0.5:0.5:5, and measuring the caking property index of the mixture, wherein the caking property index is defined as the nonstandard caking property index of the long flame coal; the product, raw flame coal, fat coal, and standard anthracite coal were mixed in a mass ratio of 0.1:0.4:0.5:5, and the nonstandard caking index of the mixture was measured.
The invention has the beneficial effects that:
1. The invention utilizes the interaction between the ionic liquid and the low-rank coal to obtain the extract containing aromatic rings, and then utilizes the beta molecular sieve to catalyze the extract, thereby increasing the fatty carbon chain of the extract and further improving the H/C ratio of the extract. The alkylated extract has moderate branching degree and aromatic ring number, and is a precursor of the coal bonding component. Through investigation of the structure and composition of the extracts and alkylated extracts, the structural and compositional characteristics of the precursor of the coal binding component can be revealed.
2. The method is green and environment-friendly in process, easy to control and simple to operate.
3. The precursor of the coal bonding component prepared by the invention obviously increases the cohesiveness of the non-caking long-flame coal, can promote the knowledge of the molecular structure of the coal bonding component, and can provide theoretical guidance for improving the quality of coke and saving coking coal sources.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1:
a method of preparing a precursor of a coal cementitious component comprising the steps of:
1) Pulverizing and sieving air-dried long flame coal and fat coal to obtain granular samples, and sealing and preserving for later use;
2) Uniformly mixing 5g of long flame coal obtained in the step 1), 3g of tributyl methyl ammonium chloride ionic liquid and 20ml of toluene solution, heating in a hydrothermal kettle at 160 ℃ for 6 hours, and cooling to room temperature to obtain a sample I;
3) Transferring the sample prepared in the step 2) into a centrifuge tube, centrifuging for 4min at a speed of 8000r/min, collecting upper liquid, adding fresh toluene (20 ml) into residual coal, performing ultrasonic oscillation for 5min, continuing centrifugal separation according to the centrifugal speed, cleaning for several times by the method until the upper liquid is nearly colorless, and recording filtrate as a sample II;
4) Carrying out reduced pressure rotary evaporation treatment on the second sample obtained in the step 3) at 55 ℃ for 20min to remove toluene, then adding absolute ethyl alcohol, carrying out reduced pressure rotary evaporation twice to sufficiently remove toluene, then adding distilled water, transferring a suspension formed by the extract, the ionic liquid and the distilled water into a centrifuge tube, centrifuging for 4min at a speed of 8000r/min, collecting a lower solid, and vacuum drying the lower solid to obtain the extract, and marking the extract as a third sample; the collected upper liquid can be recycled after rotary evaporation, and the ionic liquid can be reused.
5) Placing the beta molecular sieve in a cupel, calcining for 2 hours at 550 ℃ in an air atmosphere by using a muffle furnace to remove the template agent, adding the sample III into a hydrothermal kettle, using toluene as a solvent and using n-heptane and n-butanol as alkylation solvents, respectively adding 5g, 10g and 5g, adding 0.3g of activated beta molecular sieve, and reacting for 4 hours at 150 ℃. The reaction product was collected by centrifugation, the molecular sieve was washed with toluene until clear, the centrifugate was spin distilled, toluene and the alkylating solvent were removed, and the alkylated extract was collected and designated sample four.
6) Further, the effect of sample four obtained in step 5 on the adhesion of raw long flame coal was measured. Because the raw long flame coal has no caking property, the mass ratio of the raw long flame coal to the fat coal to the standard anthracite is 0.5:0.5:5, the caking index of the mixture was determined and defined as the nonstandard caking index for long flame coal. Sample IV, raw flame coal, fat coal and standard anthracite are mixed according to the mass ratio of 0.1:0.4:0.5:5 mixing and determining the nonstandard cohesiveness index of the mixture.
The nonstandard caking index of the long flame coal added to the alkylated extract was increased by 95% as compared to the original long flame coal.
Example 2:
Unlike example 1, example 2, step 5) is: placing the beta molecular sieve in a cupel, calcining for 2 hours at 550 ℃ in an air atmosphere by using a muffle furnace to remove the template agent, adding the sample III into a hydrothermal kettle, using toluene as a solvent and using n-heptane and n-butanol as alkylation solvents, respectively adding 5g, 10g and 5g, adding 0.3g of activated beta molecular sieve, and reacting for 4 hours at 170 ℃. The reaction product was collected by centrifugation, the molecular sieve was washed with toluene until clear, the centrifugate was spin distilled, toluene and the alkylating solvent were removed, and the alkylated extract was collected and designated sample four.
The nonstandard caking index of the long flame coal added to the alkylated extract was increased by 104% as compared to the original long flame coal.
Example 3:
Unlike example 1, example 3, step 5) is: placing the beta molecular sieve in a cupel, calcining for 2 hours at 550 ℃ in an air atmosphere by using a muffle furnace to remove the template agent, adding the sample III into a hydrothermal kettle, using toluene as a solvent and using n-heptane and n-butanol as alkylation solvents, respectively adding 5g, 10g and 5g, adding 0.3g of activated beta molecular sieve, and reacting for 4 hours at 190 ℃. The reaction product was collected by centrifugation, the molecular sieve was washed with toluene until clear, the centrifugate was spin distilled, toluene and the alkylating solvent were removed, and the alkylated extract was collected and designated sample four.
The non-standard caking index of the long flame coal incorporating the alkylated extract was increased by 159% as compared to the original long flame coal.
Example 4:
Unlike example 1, example 4, step 5) is: placing the beta molecular sieve in a cupel, calcining for 2 hours at 550 ℃ in an air atmosphere by using a muffle furnace to remove the template agent, adding the sample III into a hydrothermal kettle, using toluene as a solvent and using n-heptane and n-butanol as alkylation solvents, respectively adding 5g, 10g and 5g, adding 0.3g of activated beta molecular sieve, and reacting for 4 hours at 210 ℃. The reaction product was collected by centrifugation, the molecular sieve was washed with toluene until clear, the centrifugate was spin distilled, toluene and the alkylating solvent were removed, and the alkylated extract was collected and designated sample four.
The nonstandard caking index of the long flame coal added to the alkylated extract was increased by 129% as compared to the original long flame coal.
Example 5:
Unlike example 3, example 5, step 2) is: uniformly mixing 5g of long flame coal obtained in the step 1), 3g of tributyl methyl ammonium chloride ionic liquid and 20ml of toluene solution, heating in a hydrothermal kettle at 140 ℃ for 6 hours, and cooling to room temperature to obtain a sample I;
the non-standard caking index of the long flame coal incorporating the alkylated extract was increased by 121% as compared to the original long flame coal.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.
Claims (6)
1. A method of preparing a precursor of a coal cementitious component comprising the steps of:
1) Respectively crushing and sieving air-dried long flame coal and fat coal to obtain granular samples, and sealing and preserving for later use;
2) Uniformly mixing 5g of long flame coal obtained in the step 1), 3g of tributyl methyl ammonium chloride ionic liquid and 20ml of toluene solution, heating at a certain temperature for a certain time, and cooling to room temperature to obtain a sample I;
3) Transferring the sample prepared in the step 2) into a centrifuge tube, centrifuging for 4min at a speed of 8000r/min, collecting upper liquid, adding 20ml of fresh toluene into residual coal, performing ultrasonic oscillation for 5min, continuing centrifugal separation according to the centrifugal speed, cleaning for several times by the method until the upper liquid is nearly colorless, and recording filtrate as a sample II;
4) Carrying out reduced pressure rotary evaporation treatment on the second sample obtained in the step 3) at 55 ℃ for 20min to remove toluene, then adding absolute ethyl alcohol, carrying out reduced pressure rotary evaporation twice to sufficiently remove toluene, then adding distilled water, transferring a suspension formed by the extract, the ionic liquid and the distilled water into a centrifuge tube, centrifuging for 4min at a speed of 8000r/min, collecting a lower solid, and vacuum drying the lower solid to obtain the extract, and marking the extract as a third sample;
5) Adding the sample III into a hydrothermal kettle, adding 5g of toluene as a solvent, 10g of n-heptane and 5g of n-butanol as an alkylating solvent, adding 0.3g of activated beta molecular sieve, and reacting for 4 hours at a set temperature; and centrifugally collecting reaction products, washing the molecular sieve until the molecular sieve is transparent by using toluene, and rotationally steaming centrifugate to remove toluene and an alkylation solvent to obtain the product.
2. The method for preparing a precursor of a coal cementitious component as set forth in claim 1, wherein the reaction parameters of step 2) are: heating in a hydrothermal kettle at 70-160deg.C for 6-24 hr.
3. The method for preparing a precursor of a coal binding component according to claim 1, wherein the supernatant liquid collected by centrifugation in step 3) is subjected to rotary evaporation to recover the ionic liquid for reuse.
4. A method for preparing a precursor of a coal cementitious component as claimed in claim 1 wherein in step 5) the alkylation temperature is 150-190 ℃.
5. A method of preparing a precursor of a coal cementitious component as in claim 1 wherein the beta molecular sieve in step 5) is activated by: and placing the beta molecular sieve in a cupel, and calcining for 2 hours in an air atmosphere at 550 ℃ by using a muffle furnace to remove the template agent, so as to obtain the activated beta molecular sieve.
6. A method for preparing a precursor of a coal cementitious component according to claim 1, wherein to verify the cementitious properties of the product, the effect of the product on the raw flame coal cementitious properties is determined as follows:
Because the raw flame coal has no caking property, mixing the raw flame coal, fat coal and standard anthracite at a mass ratio of 0.5:0.5:5, and measuring the caking property index of the mixture, wherein the caking property index is defined as the nonstandard caking property index of the long flame coal; the product, raw flame coal, fat coal, and standard anthracite coal were mixed in a mass ratio of 0.1:0.4:0.5:5, and the nonstandard caking index of the mixture was measured.
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