CN107265444B - A kind of complexes and method that graphene is prepared using jet - Google Patents
A kind of complexes and method that graphene is prepared using jet Download PDFInfo
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- CN107265444B CN107265444B CN201710468891.7A CN201710468891A CN107265444B CN 107265444 B CN107265444 B CN 107265444B CN 201710468891 A CN201710468891 A CN 201710468891A CN 107265444 B CN107265444 B CN 107265444B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 179
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 106
- 238000000034 method Methods 0.000 title claims abstract description 26
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 71
- 239000010439 graphite Substances 0.000 claims abstract description 71
- 239000000463 material Substances 0.000 claims abstract description 69
- 230000007246 mechanism Effects 0.000 claims abstract description 63
- 238000001694 spray drying Methods 0.000 claims abstract description 51
- 238000005086 pumping Methods 0.000 claims abstract description 42
- 239000000243 solution Substances 0.000 claims abstract description 31
- 238000001035 drying Methods 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims description 41
- 239000011259 mixed solution Substances 0.000 claims description 38
- 239000007788 liquid Substances 0.000 claims description 25
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- 238000007599 discharging Methods 0.000 claims description 24
- 230000001133 acceleration Effects 0.000 claims description 22
- 238000001704 evaporation Methods 0.000 claims description 14
- 230000008020 evaporation Effects 0.000 claims description 14
- 239000011268 mixed slurry Substances 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- 238000010008 shearing Methods 0.000 claims description 11
- 150000001336 alkenes Chemical class 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 238000000889 atomisation Methods 0.000 claims description 7
- 238000009689 gas atomisation Methods 0.000 claims description 7
- 239000000523 sample Substances 0.000 claims description 7
- 239000004094 surface-active agent Substances 0.000 claims description 7
- 238000002604 ultrasonography Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 239000002002 slurry Substances 0.000 claims description 2
- 238000004227 thermal cracking Methods 0.000 claims description 2
- 230000000149 penetrating effect Effects 0.000 claims 1
- 238000000527 sonication Methods 0.000 claims 1
- 238000005507 spraying Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 15
- 239000006185 dispersion Substances 0.000 abstract description 3
- 239000012089 stop solution Substances 0.000 abstract 1
- 239000007921 spray Substances 0.000 description 15
- 239000000138 intercalating agent Substances 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- 238000009776 industrial production Methods 0.000 description 5
- 238000011056 performance test Methods 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 239000004575 stone Substances 0.000 description 5
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000001103 potassium chloride Substances 0.000 description 3
- 235000011164 potassium chloride Nutrition 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000032798 delamination Effects 0.000 description 2
- 239000003599 detergent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- -1 graphite Alkene Chemical class 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 229920006316 polyvinylpyrrolidine Polymers 0.000 description 2
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 2
- RZYKUPXRYIOEME-UHFFFAOYSA-N CCCCCCCCCCCC[S] Chemical compound CCCCCCCCCCCC[S] RZYKUPXRYIOEME-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000001960 triggered effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
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- Carbon And Carbon Compounds (AREA)
Abstract
Description
Performance indications | 90% graphene film radial dimension | 90% graphene thickness | Yield | Charge stripping efficiency |
Embodiment one | 50-75μm | 1.3-2.2nm | 200kg/ hours | 42.5% |
Embodiment two | 50-60μm | 1.7-3.3nm | 75kg/ hours | 32.4% |
Embodiment three | 70-100μm | 1.3-3.0nm | 100kg/ hours | 34.8% |
Example IV | 75-85μm | 1.3-5.8nm | 80kg/ hours | 32.1% |
Embodiment five | 50-65μm | 2.9-5.0nm | 50kg/ hours | 48.1% |
Claims (7)
- A kind of 1. complexes that graphene is prepared using jet, it is characterised in that including:Mixing mechanism, it is made up of body, high mixed agitator and the charging adapter A and B that are arranged on the body, discharging adapter C; At least one ultrasonic probe, ultrasonic power 100-500KW are set in the organism bottom of the mixing mechanism, material is surpassed Sonication, form mixed solution;The rotating speed for keeping accelerating pumping be 800-2000rpm, by the mixed solution acceleration of ultrasound from penetrating Flow nozzle is sprayed, and graphite is further peeled off in the jet nozzle, into drying chamber;Spray drying chamber, provided with heating system;Jet nozzle, be arranged in the spray drying chamber, be connected with the discharging adapter C, discharge adapter C and jet nozzle it Between set accelerate pumping;Collecting mechanism, for collecting grapheme material;Wherein, graphite raw material and medium solution enter mixing mechanism from charging the adapter A and B respectively, are mixed by the high puddling Device is primary to be peeled off and mixes, and during by discharging adapter C, mixed solution is accelerated pumping and accelerated, and is added from jet nozzle Speed enters in spray drying chamber, and material is peeled off in jet nozzle by collision to be sprayed, into spray drying chamber, in drying chamber At a high temperature of, solution is evaporated, and obtains grapheme material, and last collecting mechanism collects graphene.
- A kind of 2. complexes that graphene is prepared using jet according to claim 1, it is characterised in that the batch mixing The a diameter of 500-800mm of body of mechanism, is highly 700-1000mm;The blade that the high mixed agitator rotates for high speed, rotation The speed turned is 500-1000rpm.
- A kind of 3. complexes that graphene is prepared using jet according to claim 1, it is characterised in that the discharging Adapter C is arranged on mixing mechanism body, and homogenizing valve is set between mixing mechanism body.
- A kind of 4. complexes that graphene is prepared using jet according to claim 1, it is characterised in that the spraying The air pressure of drying chamber is 0.08-0.12MPa, and cavity temperature is heated to 200-250 DEG C by heating system, described in mixed solution warp Jet nozzle, into the drying chamber after be heated, mixed solution atomization, liquid by evaporation obtain grapheme material.
- A kind of 5. complexes that graphene is prepared using jet according to claim 1, it is characterised in that the acceleration The speed that is pumped into of pumping is 0.3-1L/min, and the addition speed of medium solution is pumped into speed equal to acceleration pumping.
- A kind of 6. complexes that graphene is prepared using jet according to claim 1, it is characterised in that the collection Grading room is set to sort in mechanism, unqualified powder is back to charging adapter A.
- A kind of 7. method that graphene is prepared using jet, it is characterised in that prepared using the complexes described in claim 3 Graphene, comprise the following steps:(1)It is 1 to add mass ratio to charging adapter A and charging adapter B:2-10 graphite and medium solution;(2)The blade rotational speed degree for controlling high mixed agitator to be rotation at a high speed is 500-1000rpm, primary by the high mixed agitator Peel off and mix, shearing force is provided by the homogenizing valve, after the mixed solution is thinned, obtain mixed slurry, During the adapter C that discharges, mixed solution is accelerated pumping and accelerated, and is accelerated into from jet nozzle in spray drying chamber, Material is peeled off in jet nozzle by collision to be sprayed, into spray drying chamber;(3)Spray drying chamber's gas is controlled to add spout pressure to be 0.08-0.12MPa, cavity temperature is 200-250 DEG C, described mixed Close slurry and be heated gas atomization after the acceleration pumping is pumped into the drying chamber, liquid obtains graphite by evaporation Alkene material, the grapheme material is collected using collecting mechanism;Wherein, described graphite raw material is in crystalline flake graphite, expanded graphite, highly oriented graphite, thermal cracking graphite, graphite oxide At least one, the average grain diameter of the graphite raw material are less than 1 millimeter;The medium solution is the solvent liquid containing surfactant Body, wherein, surfactant is in lauryl sodium sulfate, neopelex, polyvinylpyrrolidone, 1- pyridine acids At least one, the solvent liquid is water, methanol, benzene, at least one of acetone, the surfactant and the solvent The molal weight ratio of liquid is 1:50-100.
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Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
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EP3636592A1 (en) * | 2018-10-12 | 2020-04-15 | Advanced Material Development Limited | Liquid-exfoliated nanomaterials |
CN109701471A (en) * | 2019-02-23 | 2019-05-03 | 刘桢炀 | A kind of method and system of new chemical method preparation nano material |
CN112744813B (en) * | 2019-10-30 | 2023-02-21 | 中国石油化工股份有限公司 | Graphite modification method, modified graphite prepared by method, application of modified graphite, hydrocarbon oxidation method and volatile organic compound removal method |
CN112626322B (en) * | 2020-12-11 | 2022-12-16 | 华东理工大学 | Jet flow strengthening device and method |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102249222A (en) * | 2011-07-08 | 2011-11-23 | 北京航空航天大学 | Apparatus and process for preparing graphene by the technology of cavitating jet |
CN102701190A (en) * | 2012-05-31 | 2012-10-03 | 格雷菲尼(北京)科技有限公司 | Process and method for preparing graphene in mixed solution of water and acetone |
CN105621405A (en) * | 2016-02-29 | 2016-06-01 | 成都新柯力化工科技有限公司 | Method for preparing graphene microchip material with high-pressure water jet pulverizer |
CN106564885A (en) * | 2016-10-20 | 2017-04-19 | 成都新柯力化工科技有限公司 | Jet device for continuous preparation of graphene and method thereof |
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2017
- 2017-06-20 CN CN201710468891.7A patent/CN107265444B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102249222A (en) * | 2011-07-08 | 2011-11-23 | 北京航空航天大学 | Apparatus and process for preparing graphene by the technology of cavitating jet |
CN102701190A (en) * | 2012-05-31 | 2012-10-03 | 格雷菲尼(北京)科技有限公司 | Process and method for preparing graphene in mixed solution of water and acetone |
CN105621405A (en) * | 2016-02-29 | 2016-06-01 | 成都新柯力化工科技有限公司 | Method for preparing graphene microchip material with high-pressure water jet pulverizer |
CN106564885A (en) * | 2016-10-20 | 2017-04-19 | 成都新柯力化工科技有限公司 | Jet device for continuous preparation of graphene and method thereof |
Non-Patent Citations (1)
Title |
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射流空化方法制备石墨烯研究;沈志刚等;《颗粒学最新进展研讨会——暨第十届全国颗粒制备与处理研讨会》;20111130;第54页倒数第2段 * |
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