CN106554012A - The preparation method of modified superfine Graphene - Google Patents
The preparation method of modified superfine Graphene Download PDFInfo
- Publication number
- CN106554012A CN106554012A CN201610888941.2A CN201610888941A CN106554012A CN 106554012 A CN106554012 A CN 106554012A CN 201610888941 A CN201610888941 A CN 201610888941A CN 106554012 A CN106554012 A CN 106554012A
- Authority
- CN
- China
- Prior art keywords
- graphene
- kneading
- pasty material
- preparation
- superfine
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 20
- 239000002245 particle Substances 0.000 claims abstract description 18
- 238000004898 kneading Methods 0.000 claims abstract description 16
- 235000011837 pasties Nutrition 0.000 claims abstract description 16
- -1 graphite alkene Chemical class 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 9
- 239000010439 graphite Substances 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 9
- 238000000605 extraction Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 239000012141 concentrate Substances 0.000 claims abstract description 4
- 238000000703 high-speed centrifugation Methods 0.000 claims abstract description 4
- 150000002148 esters Chemical class 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 10
- 229920000642 polymer Polymers 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 9
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 6
- TZBAVQKIEKDGFH-UHFFFAOYSA-N n-[2-(diethylamino)ethyl]-1-benzothiophene-2-carboxamide;hydrochloride Chemical compound [Cl-].C1=CC=C2SC(C(=O)NCC[NH+](CC)CC)=CC2=C1 TZBAVQKIEKDGFH-UHFFFAOYSA-N 0.000 claims description 6
- 229920000058 polyacrylate Polymers 0.000 claims description 6
- 229940093430 polyethylene glycol 1500 Drugs 0.000 claims description 6
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 5
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 5
- 239000004094 surface-active agent Substances 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 229920002319 Poly(methyl acrylate) Polymers 0.000 claims description 3
- 229920001273 Polyhydroxy acid Polymers 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 229920006243 acrylic copolymer Polymers 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- 229910052593 corundum Inorganic materials 0.000 claims description 3
- 239000010431 corundum Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000002736 nonionic surfactant Substances 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 3
- 229920000344 molecularly imprinted polymer Polymers 0.000 claims description 2
- 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 claims 1
- 239000004743 Polypropylene Substances 0.000 claims 1
- 229920001155 polypropylene Polymers 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 230000003750 conditioning effect Effects 0.000 abstract description 4
- 239000008187 granular material Substances 0.000 description 3
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- 229920002125 Sokalan® Polymers 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000004702 methyl esters Chemical class 0.000 description 2
- 239000004584 polyacrylic acid Substances 0.000 description 2
- 230000004308 accommodation Effects 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000003913 materials processing Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000004575 stone Substances 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
- C01B2204/20—Graphene characterized by its properties
-
- 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
Landscapes
- Cosmetics (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of preparation method of modified superfine Graphene, comprises the steps：(1) grind：First Graphene is placed in grinder, grinding obtains Graphene pasty material；(2) staged care：Graphene pasty material is put in high speed centrifugation decanter type grader, the Graphene pasty material of wherein particle diameter≤1 μm concentrates on the middle part of grader, deposits in storage tank after extraction；(3) kneading is processed：The Graphene pasty material of particle diameter≤1 μm is put in kneading consersion unit, addition surface conditioning agent carries out kneading process, superfine graphite alkene powder body is obtained after kneading, period, the bulk density of superfine graphite alkene powder body is controlled 0.5 1.2.Have dispersive property good using modified superfine graphene particles obtained in the present invention, the low characteristic of bulk density, to electromagnetic wave and the shadow shield of wireless signal energy and interference, reaches the effect got the mastery in information competition.
Description
Technical field
The present invention relates to a kind of preparation method of modified superfine Graphene.
Background technology
Haze is a kind of natural phenomena of atmospheric pollution, and the granule in haze is generally PM2.5, i.e. particle diameter 2.5
Micron is following.According to this phenomenon, the materials processing disturbed with anti-electromagnetic wave and signal can be become particle diameter 1-2 microns
Hereinafter, the mist of aeroge can by appropriate process for treating surface, be formed in an atmosphere with the air-flow in air and hydrone
Haze.As these granules all have an effect of interference electromagnetic wave, the haze for being formed just be provided with desired anti-electromagnetic wave and
The effect of signal interference, this can play a role for winning information war.
But at present, the particle dispersion of such artificial haze can be poor, and bulk density is higher, and surface mobility is poor, causes
The ability of its anti-electromagnetic wave and signal interference is weaker.
The content of the invention
The purpose of the present invention is can be poor to solve the particle dispersion of artificial haze at present, and bulk density is higher, surface
Poor fluidity, the technical problem for causing the ability that its anti-electromagnetic wave and signal are disturbed weaker.
In order to solve above-mentioned technical problem, the present invention provides a kind of preparation method of modified superfine Graphene, including as follows
Step：
(1) grind：First Graphene is placed in grinder, deionized water is added, then is added hyper-dispersant, in the work that mill is situated between
With lower grinding 20 hours, Graphene pasty material is obtained；
(2) staged care：The Graphene pasty material is put in high speed centrifugation decanter type grader, wherein particle diameter≤
1 μm of Graphene pasty material concentrates on the middle part of grader, deposits in storage tank after extraction；The Graphene slurry that 1 μm of particle diameter ＞
Shape material is concentrated on the outside of grader, continues grinding in returning grinder after extraction；
(3) kneading is processed：The Graphene pasty material of particle diameter≤1 μm is put in kneading consersion unit, adds table
Face inorganic agent carries out kneading process, and superfine graphite alkene powder body, period, by the accumulation of the superfine graphite alkene powder body are obtained after kneading
Density domination is in 0.5-1.2.
Further, hyper-dispersant described in step (1) be acrylic copolymer, the trade mark be CH-10B, CH18, CH-7,
One kind in the hyper-dispersant of CH13E, or mixture more than two of which.
Further, surface conditioning agent described in step (3) is low-carbon (LC) polyhydroxy-alcohol, Long carbon chain unit alcohol, Long carbon chain list
First acid, low-carbon (LC) polyhydroxy acid, organic amine surfactant, esters surface active agent, nonionic surfactant, hydroxyl
High molecular polymer and its esters and carboxylic high molecular polymer and the one kind in its esters, or it is more than two of which mixed
Compound.
Further, the high molecular polymer and its esters of the hydroxyl be polyethylene glycol 1500, Macrogol 4000,
One kind in polymethyl acrylate, butyl polyacrylate and sodium polyacrylate, or mixture more than two of which；
The carboxylic high molecular polymer and its esters are polyethylene glycol 1500, Macrogol 4000, polyacrylic acid
One kind in methyl ester, butyl polyacrylate and sodium polyacrylate, or mixture more than two of which.
Further, by zirconium oxide or corundum made by ball of mill Jie described in step (1) for diameter 0.5-3 millimeters.
Using modified superfine graphene particles particle diameter≤1 μm obtained in the present invention, then surface coated process is carried out to which,
So that ultra-fine grapheme material obtains fully dispersed, bulk density low characteristic good with dispersive property；Then it is these are straight
Footpath much smaller than PM2.5 ultra-fine grain pack after be supplied to aircraft, as the belongings of aircraft, required upper
There is explosion or sprinkling in empty or place so that these ultra-fine granules form a kind of aerosol state or haze in the air with air
Guard, shadow shield and interference are carried out to location electromagnetic wave and wireless signal, are reached and is got the mastery in information competition
Effect.
Specific embodiment
Presently in connection with embodiment, the present invention is further detailed explanation, and application of the invention is not limited to following
Embodiment, falls within protection scope of the present invention to any pro forma accommodation done by the present invention.
The preparation method of the modified superfine Graphene of the present invention, comprises the steps：
(1) grind：First Graphene is placed in grinder, add 500 milliliters of deionized water, then add the trade mark for CH18,
The hyper-dispersant of CH-7 is each 0.25 gram, is that the zirconium oxide of 0.5-3mm or ball made by corundum grind 20 hours by sphere diameter, obtains stone
Black alkene pasty material；
(2) staged care：The Graphene pasty material is put in high speed centrifugation decanter type grader, wherein particle diameter≤
1 μm of Graphene pasty material concentrates on the middle part of grader, deposits in storage tank after extraction；The Graphene slurry that 1 μm of particle diameter ＞
Shape material is concentrated on the outside of grader, continues grinding in returning grinder after extraction；
(3) kneading is processed：The Graphene pasty material of particle diameter≤1 μm is put in kneading consersion unit, addition
The surface conditioning agent of 0.2-2.0wt% carries out kneading process, and preferred surface inorganic agent consumption is 0.5wt%, mediates process time
For 25 hours, superfine graphite alkene powder body is obtained after kneading, period, the bulk density control of the superfine graphite alkene powder body is existed
0.5-1.2；Superfine graphite alkene powder body yield up to standard reaches 60Wt% or so.
Preferably, hyper-dispersant described in step (1) be acrylic copolymer, the trade mark be CH-10B, CH18, CH-7,
One kind in the hyper-dispersant of CH13E, or mixture more than two of which.
Preferably, surface conditioning agent described in step (3) is low-carbon (LC) polyhydroxy-alcohol, Long carbon chain unit alcohol, Long carbon chain unit
Acid, low-carbon (LC) polyhydroxy acid, organic amine surfactant, esters surface active agent, nonionic surfactant, the height of hydroxyl
Molecularly Imprinted Polymer and its esters and carboxylic high molecular polymer and the one kind in its esters, or mixing more than two of which
Thing.
Preferably, the high molecular polymer and its esters of the hydroxyl is polyethylene glycol 1500, Macrogol 4000, gathers
One kind in acrylic acid methyl ester., butyl polyacrylate and sodium polyacrylate, or mixture more than two of which；
The carboxylic high molecular polymer and its esters are polyethylene glycol 1500, Macrogol 4000, polyacrylic acid
One kind in methyl ester, butyl polyacrylate and sodium polyacrylate, or mixture more than two of which.
With the above-mentioned desirable embodiment according to the present invention as enlightenment, by above-mentioned description, relevant staff is complete
Various change and modification can be carried out in the range of without departing from this invention technological thought entirely.The technology of this invention
Property scope is not limited to the content in description, it is necessary to its technical scope is determined according to right.
Claims (5)
1. the preparation method of modified superfine Graphene, it is characterised in that comprise the steps：
(1) grind：First Graphene is placed in grinder, deionized water is added, then is added hyper-dispersant, in the presence of mill is situated between
Grinding 20 hours, obtains Graphene pasty material；
(2) staged care：The Graphene pasty material is put in high speed centrifugation decanter type grader, wherein particle diameter≤1 μm
Graphene pasty material concentrate on the middle part of grader, deposit in storage tank after extraction；The Graphene slurry of 1 μm of particle diameter ＞
Material is concentrated on the outside of grader, continues grinding in returning grinder after extraction；
(3) kneading is processed：The Graphene pasty material of particle diameter≤1 μm is put in kneading consersion unit, at addition surface
Reason agent carries out kneading process, and superfine graphite alkene powder body, period, by the bulk density of the superfine graphite alkene powder body are obtained after kneading
Control is in 0.5-1.2.
2. the preparation method of modified superfine Graphene according to claim 1, it is characterised in that surpass described in step (1)
One kind in the hyper-dispersant that dispersant is acrylic copolymer, the trade mark is CH-10B, CH18, CH-7, CH13E, or wherein two
Plant the mixture of the above.
3. the preparation method of modified superfine Graphene according to claim 2, it is characterised in that table described in step (3)
Face inorganic agent is low-carbon (LC) polyhydroxy-alcohol, Long carbon chain unit alcohol, the acid of Long carbon chain unit, low-carbon (LC) polyhydroxy acid, the work of organic amine surface
Property agent, esters surface active agent, nonionic surfactant, the high molecular polymer of hydroxyl and its esters and carboxylic height
One kind in Molecularly Imprinted Polymer and its esters, or mixture more than two of which.
4. the preparation method of modified superfine Graphene according to claim 3, it is characterised in that the high score of the hydroxyl
Sub- polymer and its esters are polyethylene glycol 1500, Macrogol 4000, polymethyl acrylate, butyl polyacrylate and polypropylene
One kind in sour sodium, or mixture more than two of which；
The carboxylic high molecular polymer and its esters be polyethylene glycol 1500, Macrogol 4000, polymethyl acrylate,
One kind in butyl polyacrylate and sodium polyacrylate, or mixture more than two of which.
5. the preparation method of modified superfine Graphene according to claim 1, it is characterised in that grind described in step (1)
The ball by made by zirconium oxide or corundum being situated between for diameter 0.5-3 millimeters.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610888941.2A CN106554012B (en) | 2016-10-11 | 2016-10-11 | The preparation method of modified superfine graphene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610888941.2A CN106554012B (en) | 2016-10-11 | 2016-10-11 | The preparation method of modified superfine graphene |
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| Publication Number | Publication Date |
|---|---|
| CN106554012A true CN106554012A (en) | 2017-04-05 |
| CN106554012B CN106554012B (en) | 2018-09-28 |
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| CN201610888941.2A Active CN106554012B (en) | 2016-10-11 | 2016-10-11 | The preparation method of modified superfine graphene |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109533267A (en) * | 2018-12-25 | 2019-03-29 | 哈尔滨工业大学 | A kind of Hengsheng power inflation closed pore micro-structure floating material cell |
| CN110453302A (en) * | 2019-04-19 | 2019-11-15 | 陕西金瑞烯科技发展有限公司 | A kind of preparation method of graphene nylon fibre |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1244495A (en) * | 1998-08-10 | 2000-02-16 | 张小宁 | Preparation of superfine graphite powder |
| CN104194455A (en) * | 2014-08-25 | 2014-12-10 | 鸿纳（东莞）新材料科技有限公司 | Graphene coating as well as preparation method and coating method thereof |
| CN105084345A (en) * | 2014-04-28 | 2015-11-25 | 宁波墨西科技有限公司 | Graphene material powder and preparation method |
-
2016
- 2016-10-11 CN CN201610888941.2A patent/CN106554012B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1244495A (en) * | 1998-08-10 | 2000-02-16 | 张小宁 | Preparation of superfine graphite powder |
| CN105084345A (en) * | 2014-04-28 | 2015-11-25 | 宁波墨西科技有限公司 | Graphene material powder and preparation method |
| CN104194455A (en) * | 2014-08-25 | 2014-12-10 | 鸿纳（东莞）新材料科技有限公司 | Graphene coating as well as preparation method and coating method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109533267A (en) * | 2018-12-25 | 2019-03-29 | 哈尔滨工业大学 | A kind of Hengsheng power inflation closed pore micro-structure floating material cell |
| CN109533267B (en) * | 2018-12-25 | 2022-01-25 | 哈尔滨工业大学 | Constant-lift inflatable closed-cell micro-structure floating material unit |
| CN110453302A (en) * | 2019-04-19 | 2019-11-15 | 陕西金瑞烯科技发展有限公司 | A kind of preparation method of graphene nylon fibre |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106554012B (en) | 2018-09-28 |
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Effective date of registration: 20231020 Address after: No.21 Xingda Road, Touqiao Town, Guangling District, Yangzhou City, Jiangsu Province, 225000 Patentee after: Jiangsu Youchuang Photoelectric Technology Co.,Ltd. Address before: 225100 No.1, No.8, Huagang Road, Hanjiang Industrial Park, Hanjiang District, Yangzhou City, Jiangsu Province Patentee before: JIANGSU HUALI SUOFEI NEW MATERIAL CO.,LTD. |