CN108975323A - graphene oxide cleaning method - Google Patents
graphene oxide cleaning method Download PDFInfo
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- CN108975323A CN108975323A CN201811029177.9A CN201811029177A CN108975323A CN 108975323 A CN108975323 A CN 108975323A CN 201811029177 A CN201811029177 A CN 201811029177A CN 108975323 A CN108975323 A CN 108975323A
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- graphene oxide
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- rotary washer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/198—Graphene oxide
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Abstract
Graphene oxide cleaning method, it is related to a kind of graphene oxide cleaning method, the preparation field of graphene oxide.The present invention is to solve the technical problem that the washing cycle of graphene oxide is grown.This method is as follows: the graphene oxide slurry that material content is 0.1%~0.5% being injected rotary washer with lining tetrafluoro centrifugal pump, it is recycled what is isolated containing acid, salt bearing liquid wastes by accumulator tank, deionized water is injected into rotary washer, the slurry after cleaning is diluted, and rotary-cleaning again, scrub raffinate is discharged, total wash time introduces rotary washer using dedusting compressed air for 12h, the material blowback that will be isolated, the graphene oxide after being cleaned.It is an advantage of the invention that saving water, being easy to operate, washing cycle and material washing quality are shortened.Washing cycle of the invention is 12h.
Description
Technical field
The present invention relates to a kind of graphene oxide cleaning method, the preparation fields of graphene oxide.
Background technique
When Hummers method prepares graphene oxide, when a certain proportion of concentrated sulfuric acid, potassium permanganate, crystalline flake graphite raw material
Reaction is completed, and after being diluted with water, is needed the graphene oxide product obtained washing, separation from acid solution.It is well known that
Since surface of graphene oxide has a large amount of oxygen-containing hydrophilic functional groups, and graphene oxide size is tiny, prepares the sulphur in stoste
Acid group, manganese salt etc. are difficult to filter out, and the washing and separation of oxidizing graphene create great difficulties, and cause washing cycle long.
Currently, the separation and cleaning problem of graphene oxide, are huge Pinch technology problems present in graphene industrial production.
Summary of the invention
The purpose of the present invention is to solve the technical problems that the washing cycle of graphene oxide is long, provide a kind of oxidation
Graphene cleaning method.
Graphene oxide cleaning method follows the steps below:
One, the graphene oxide slurry that material content is 0.1%~0.5% is injected with lining tetrafluoro centrifugal pump rotary clear
Device is washed, is recycled what is isolated containing acid, salt bearing liquid wastes by accumulator tank；
Two, deionized water is injected into rotary washer, the slurry after cleaning is diluted, and rotary-cleaning again,
Scrub raffinate is discharged；
Three, it repeats step 2 3~6 times；
Four, total wash time of step 1 to step 3 is 12h, using the dedusting compressed air of 0.1MPa~0.5MPa,
Rotary washer is introduced, the material blowback that will be isolated, the graphene oxide after being cleaned.
Based on problem present on graphene oxide cleaning, it is contemplated that existing cleaning method is protected in preparation efficiency, environment
Deficiency existing in terms of shield and economic benefit, the invention proposes a kind of new graphene oxide cleaning processes, by the oxygen of acquisition
Graphite alkene dispersion liquid is dry, and by thermal reduction, can get graphene product.The cleaning device that this method uses, acid oxygen
Graphite alkene slurry removes the impurity such as acid and the salt in solution, obtains neutral alumina graphene through flushing, filtering, backwash etc.
Dispersion liquid.
The technical scheme adopted by the invention is that:
1. using rotary filtering device.
2. being changed to original deionized water back flush mode using compressed air blowback.
Acid solution after 3 cleanings is recycled using recycling can.
4 washing mediums of the present invention are deionized water, and backflushing medium is dedusting compressed air.
It is an advantage of the invention that saving water, being easy to operate, washing cycle and material washing quality are shortened.Of the invention
Washing cycle is 12h.
Specific embodiment
The technical solution of the present invention is not limited to the following list, further includes between each specific embodiment
Any combination.
Specific embodiment 1: present embodiment graphene oxide cleaning method follows the steps below:
One, the graphene oxide slurry that material content is 0.1%~0.5% is injected with lining tetrafluoro centrifugal pump rotary clear
Device is washed, recycling can is recycled to by accumulator tank containing acid, salt bearing liquid wastes by what is isolated；
Two, deionized water is injected into rotary washer, the slurry after cleaning is diluted, and rotary-cleaning again,
Scrub raffinate is discharged；
Three, it repeats step 2 3~6 times；
Four, total wash time of step 1 to step 3 is 12h, using the dedusting compressed air of 0.1MPa~0.5MPa,
Rotary washer is introduced, the material blowback that will be isolated, the graphene oxide after being cleaned.
Specific embodiment 2: the present embodiment is different from the first embodiment in that material content described in step 1
Rotary washer is injected for 0.25% graphene oxide slurry.It is other same as the specific embodiment one.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that material described in step 1
The graphene oxide slurry that content is 0.2% injects rotary washer.It is other the same as one or two specific embodiments.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three described in step 1
The graphene oxide slurry that material content is 0.3% injects rotary washer.One of other and specific embodiment one to three
It is identical.
Specific embodiment 5: being repeated in step 3 unlike one of present embodiment and specific embodiment one to four
Step 24 times.It is other identical as one of specific embodiment one to four.
Specific embodiment 6: being used in step 4 unlike one of present embodiment and specific embodiment one to five
The dedusting compressed air of 0.2MPa, introduces rotary washer.It is other identical as one of specific embodiment one to five.
Specific embodiment 7: being used in step 4 unlike one of present embodiment and specific embodiment one to six
The dedusting compressed air of 0.3MPa, introduces rotary washer.It is other identical as one of specific embodiment one to six.
Specific embodiment 8: being used in step 4 unlike one of present embodiment and specific embodiment one to seven
The dedusting compressed air of 0.4MPa, introduces rotary washer.It is other identical as one of specific embodiment one to seven.
Specific embodiment 9: unlike one of present embodiment and specific embodiment one to eight described in step 1
Material in rotary washer is microporous membrane.It is other identical as one of specific embodiment one to eight.
Effect of the present invention is verified using following embodiments:
Embodiment 1:
Graphene oxide cleaning method follows the steps below:
One, the graphene oxide slurry that material content is 0.1% is injected into rotary washer with lining tetrafluoro centrifugal pump, it will
That isolates is recycled containing acid, salt bearing liquid wastes by accumulator tank；
Two, deionized water is injected into rotary washer, the slurry after cleaning is diluted, and rotary-cleaning again,
Scrub raffinate is discharged；
Three, it repeats step 23 times；
Four, total wash time of step 1 to step 3 is 12h, using the dedusting compressed air of 0.1MPa, introduces rotation
Formula washer, the material blowback that will be isolated, the graphene oxide after being cleaned.
The present embodiment washing cycle is 12h.
Embodiment 2:
Graphene oxide cleaning method follows the steps below:
One, the graphene oxide slurry that material content is 0.2% is injected into rotary washer with lining tetrafluoro centrifugal pump, it will
That isolates is recycled containing acid, salt bearing liquid wastes by accumulator tank；
Two, deionized water is injected into rotary washer, the slurry after cleaning is diluted, and rotary-cleaning again,
Scrub raffinate is discharged；
Three, it repeats step 24 times；
Four, total wash time of step 1 to step 3 is 12h, using the dedusting compressed air of 0.3MPa, introduces rotation
Formula washer, the material blowback that will be isolated, the graphene oxide after being cleaned.
The present embodiment washing cycle is 12h.
Embodiment 3:
Graphene oxide cleaning method follows the steps below:
One, the graphene oxide slurry that material content is 0.25% is injected into rotary washer with lining tetrafluoro centrifugal pump,
It is recycled what is isolated containing acid, salt bearing liquid wastes by accumulator tank；
Two, deionized water is injected into rotary washer, the slurry after cleaning is diluted, and rotary-cleaning again,
Scrub raffinate is discharged；
Three, it repeats step 26 times；
Four, total wash time of step 1 to step 3 is 12h, using the dedusting compressed air of 0.2MPa, introduces rotation
Formula washer, the material blowback that will be isolated, the graphene oxide after being cleaned.
The present embodiment washing cycle is 12h.
Claims (9)
1. graphene oxide cleaning method, it is characterised in that graphene oxide cleaning method follows the steps below:
One, the rotary cleaning of graphene oxide slurry injection for being 0.1%~0.5% by material content with lining tetrafluoro centrifugal pump
Device is recycled what is isolated containing acid, salt bearing liquid wastes by accumulator tank；
Two, deionized water is injected into rotary washer, the slurry after cleaning is diluted with deionized water, and rotates again
Scrub raffinate is discharged in cleaning；
Three, it repeats step 2 3~6 times；
Four, total wash time of step 1 to step 3 is 12h, using the dedusting compressed air of 0.1MPa~0.5MPa, is introduced
Rotary washer, the material blowback that will be isolated, the graphene oxide after being cleaned.
2. graphene oxide cleaning method according to claim 1, it is characterised in that material content described in step 1 is
0.25% graphene oxide slurry injects rotary washer.
3. graphene oxide cleaning method according to claim 1, it is characterised in that material content described in step 1 is
0.2% graphene oxide slurry injects rotary washer.
4. graphene oxide cleaning method according to claim 1, it is characterised in that material content described in step 1 is
0.3% graphene oxide slurry injects rotary washer.
5. graphene oxide cleaning method according to claim 1, it is characterised in that repeated step 24 times in step 3.
6. graphene oxide cleaning method according to claim 1, it is characterised in that use the dedusting of 0.2MPa in step 4
Compressed air introduces rotary washer.
7. graphene oxide cleaning method according to claim 1, it is characterised in that use the dedusting of 0.3MPa in step 4
Compressed air introduces rotary washer.
8. graphene oxide cleaning method according to claim 1, it is characterised in that use the dedusting of 0.4MPa in step 4
Compressed air introduces rotary washer.
9. graphene oxide cleaning method according to claim 1, it is characterised in that rotary washer described in step 1
In material be microporous membrane.
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| CN201811029177.9A CN108975323A (en) | 2018-09-05 | 2018-09-05 | graphene oxide cleaning method |
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| CN201811029177.9A CN108975323A (en) | 2018-09-05 | 2018-09-05 | graphene oxide cleaning method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109437183A (en) * | 2019-01-04 | 2019-03-08 | 新疆烯金石墨烯科技有限公司 | The circulation utilization method of acid-bearing wastewater in a kind of graphene oxide postprocessing working procedures |
| CN110156004A (en) * | 2019-07-08 | 2019-08-23 | 菏泽学院 | A kind of graphene oxide cleaning device |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103066281A (en) * | 2013-01-09 | 2013-04-24 | 上海交通大学 | Synergistically modified lithium-iron-phosphate positive active material enveloped with graphene three-dimensional network and doped with metal ions and preparation method of lithium-iron-phosphate positive active material |
| CN104370286A (en) * | 2014-11-04 | 2015-02-25 | 张泽宇 | Novel graphene preparation technique |
| CN204369570U (en) * | 2014-12-08 | 2015-06-03 | 厦门烯成新材料科技有限公司 | A kind of Graphene water washing device |
| CN105063423A (en) * | 2015-08-06 | 2015-11-18 | 陆春玲 | Medical graphene enhanced titanium alloy rod |
| CN105347340A (en) * | 2015-12-14 | 2016-02-24 | 太原理工大学 | Preparation method of graphene oxide |
| WO2017190570A1 (en) * | 2016-05-06 | 2017-11-09 | 成都新柯力化工科技有限公司 | Large-scale clean preparation method for graphene |
| CN107697910A (en) * | 2017-11-24 | 2018-02-16 | 多凌新材料科技股份有限公司 | The separation of graphene oxide and method of purification |
| CN107117607B (en) * | 2017-06-20 | 2018-03-13 | 成都新柯力化工科技有限公司 | A kind of method that graphene is prepared based on ray classification stripping |
-
2018
- 2018-09-05 CN CN201811029177.9A patent/CN108975323A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103066281A (en) * | 2013-01-09 | 2013-04-24 | 上海交通大学 | Synergistically modified lithium-iron-phosphate positive active material enveloped with graphene three-dimensional network and doped with metal ions and preparation method of lithium-iron-phosphate positive active material |
| CN104370286A (en) * | 2014-11-04 | 2015-02-25 | 张泽宇 | Novel graphene preparation technique |
| CN204369570U (en) * | 2014-12-08 | 2015-06-03 | 厦门烯成新材料科技有限公司 | A kind of Graphene water washing device |
| CN105063423A (en) * | 2015-08-06 | 2015-11-18 | 陆春玲 | Medical graphene enhanced titanium alloy rod |
| CN105347340A (en) * | 2015-12-14 | 2016-02-24 | 太原理工大学 | Preparation method of graphene oxide |
| WO2017190570A1 (en) * | 2016-05-06 | 2017-11-09 | 成都新柯力化工科技有限公司 | Large-scale clean preparation method for graphene |
| CN107117607B (en) * | 2017-06-20 | 2018-03-13 | 成都新柯力化工科技有限公司 | A kind of method that graphene is prepared based on ray classification stripping |
| CN107697910A (en) * | 2017-11-24 | 2018-02-16 | 多凌新材料科技股份有限公司 | The separation of graphene oxide and method of purification |
Non-Patent Citations (3)
| Title |
|---|
| 元英进: "《现代制药工艺学》", 30 July 2004 * |
| 姜信真: "《化工生产基础知识》", 30 September 1983 * |
| 范洪远: "物理气相沉积（PVD）制备石墨类薄膜", 《中国优秀硕士学位论文全文数据库·工程科技Ⅰ辑》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109437183A (en) * | 2019-01-04 | 2019-03-08 | 新疆烯金石墨烯科技有限公司 | The circulation utilization method of acid-bearing wastewater in a kind of graphene oxide postprocessing working procedures |
| CN109437183B (en) * | 2019-01-04 | 2022-01-14 | 新疆烯金石墨烯科技有限公司 | Method for recycling acid-containing wastewater in graphene oxide post-treatment process |
| CN110156004A (en) * | 2019-07-08 | 2019-08-23 | 菏泽学院 | A kind of graphene oxide cleaning device |
| CN110156004B (en) * | 2019-07-08 | 2022-04-08 | 菏泽学院 | Oxidized graphene cleaning device |
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