CN104108707A - Sulfur-doped graphene and preparation method thereof - Google Patents
Sulfur-doped graphene and preparation method thereof Download PDFInfo
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- CN104108707A CN104108707A CN201410360674.2A CN201410360674A CN104108707A CN 104108707 A CN104108707 A CN 104108707A CN 201410360674 A CN201410360674 A CN 201410360674A CN 104108707 A CN104108707 A CN 104108707A
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Abstract
The invention relates to sulfur-doped graphene and a preparation method thereof. The preparation method comprises the following steps: heating a sulfur source and an organic salt or a mixture of organic acids and salts to 300-1600 DEG C in a non-oxidizing atmosphere, thereby obtaining a mixture of the sulfur-doped graphene and metallic oxides; removing the metallic oxide in the mixture, thereby obtaining the sulfur-doped graphene. The sulfur source and the organic salt or the mixture of organic acids and salts are heated in the non-oxidizing atmosphere, and the sulfur-doped graphene is prepared by utilizing the concept of generating active sulfur through graphene carbonization based on organic salts, inorganic oxide nucleation and sulfur source pyrolysis. The method has the advantages of simple process, short production period, capacity of performing in-situ doping, and the like, and the prepared sulfur-doped graphene has the characteristics of porosity, large specific surface area and aggregation avoidance and can be widely applied to various fields of lithium ion batteries, supercapacitors, lead-acid cells, water treatment, electro-catalysis, photocatalysis and the like.
Description
Technical field
The present invention relates to carbon material technical field, is a kind of sulfur doping Graphene and preparation method thereof specifically.
Background technology
Since the people such as Geim in 2004 successfully prepare mono-layer graphite, Graphene is with two dimension (2D) the honeycomb carbon structure of its uniqueness and excellent physics, chemistry, mechanical property, and the research of Graphene is a current study hotspot.Yet energy gap is too small in grapheme material electronic spectrum, can not as traditional semi-conductor, control by complete quilt, may stop that large switch signal compares etc.Hetero atom is incorporated into the sp of Graphene
2hybrid structure is proved to be a kind of and effectively opens Graphene band gap and improve one of method of its chemical reactivity, for its application, has great significance.
Sulfur doping Graphene is a kind of important Graphene derivative, in alkaline medium, than commercial platinum/carbon, has more excellent catalytic activity.In prior art, about preparing the method for sulfur doping Graphene, have graphene oxide to heat in hydrogen sulfide atmosphere to mix sulphur, anneal oxidation Graphene and Benzyl disulfide, thermal annealing sulfonated polystyrene film etc. in argon hydrogen atmosphere in argon gas.There is non-uniform doping, the building-up process of complexity and the poisonous shortcomings such as presoma in first two method.Last method relates to the preparation of sulfonated polystyrene, the spin coating of polymeric film, high-temperature heat treatment and a plurality of steps such as follow-up.
Summary of the invention
In order to make up above-mentioned the deficiencies in the prior art, technical problem to be solved by this invention is to provide that a kind of technique is simple, sulfur doping graphene preparation method that can in-situ doped sulphur.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is:
A sulfur doping graphene preparation method, comprising:
By sulphur source and organic salt or be heated to 300-1600 ℃ with the mixture of organic acid and salt under non-oxidizing atmosphere, obtain the mixture of sulfur doping Graphene and metal oxide;
Remove the metal oxide in mixture, obtain sulfur doping Graphene;
Wherein, described sulphur source is selected from one or more in di-n-octyl thioether, dodecyl thioether, tetramethylene sulfone, 4-propylthio vinyl acetate, sulfuric acid vinyl ester, propylene sulfite, sulfuric acid propylene, 4-methyl ethylene sulfite and butylene sulfite;
Wherein, described organic salt is selected from alkyl soap that Citrate trianion, gluconate, tartrate, D-VB5 salt, threose acid salt, the carbonatoms of magnesium, calcium, strontium, barium, cobalt, nickel, manganese, iron, zinc, aluminium, indium or bismuth are 8-24 and one or more in oleate;
Wherein, described organic acid is selected from citric acid, gluconic acid, tartrate, D-VB5, threonic acid, alkyl lipid acid that carbonatoms is 8-24 and one or more in oleic acid;
Wherein, described salt is selected from one or more in acetate, nitrate, chlorate, Bromide and the iodized salt of magnesium, calcium, strontium, barium, cobalt, nickel, manganese, iron, zinc, aluminium, indium or bismuth.
Beneficial effect of the present invention is: technique is simple, with short production cycle, can in-situ doped sulphur, the sulfur doping Graphene making has porousness, feature that specific surface area is large, can be applicable to the every field such as lithium ion battery, ultracapacitor, lead-acid cell, water treatment, electrocatalysis, photochemical catalysis.
Accompanying drawing explanation
Figure 1 shows that the scanning electron microscope (SEM) photograph of the sulfur doping Graphene of the embodiment of the present invention 1 preparation.
Embodiment
By describing technology contents of the present invention, structural attitude in detail, being realized object and effect, below in conjunction with embodiment and coordinate accompanying drawing to be explained in detail.
The design of most critical of the present invention is: by non-oxidizing atmosphere, heat sulphur source and organic salt or with the mixture of organic acid and salt; utilize organic salt carbonized graphite alkene, inorganic oxide nucleation and the pyrolysis of sulphur source to produce the theory of active sulphur; prepare the original position sulfur doping Graphene of advantages such as thering is porousness, specific surface area is large; the method technique is simple, with short production cycle, be produced on a large scale, and the sulfur doping Graphene preparing can be applicable to the every field such as lithium ion battery, ultracapacitor, lead-acid cell, water treatment, electrocatalysis, photochemical catalysis.
Sulfur doping graphene preparation method provided by the invention, comprising:
By sulphur source and organic salt or be heated to 300-1600 ℃ with the mixture of organic acid and salt under non-oxidizing atmosphere, obtain the mixture of sulfur doping Graphene and metal oxide;
Remove the metal oxide in mixture, obtain sulfur doping Graphene;
Wherein, described sulphur source is selected from one or more in di-n-octyl thioether, dodecyl thioether, tetramethylene sulfone, 4-propylthio vinyl acetate, sulfuric acid vinyl ester, propylene sulfite, sulfuric acid propylene, 4-methyl ethylene sulfite and butylene sulfite;
Wherein, described organic salt is selected from alkyl soap that Citrate trianion, gluconate, tartrate, D-VB5 salt, threose acid salt, the carbonatoms of magnesium, calcium, strontium, barium, cobalt, nickel, manganese, iron, zinc, aluminium, indium or bismuth are 8-24 and one or more in oleate;
Wherein, described organic acid is selected from citric acid, gluconic acid, tartrate, D-VB5, threonic acid, alkyl lipid acid that carbonatoms is 8-24 and one or more in oleic acid;
Wherein, described salt is selected from one or more in acetate, nitrate, chlorate, Bromide and the iodized salt of magnesium, calcium, strontium, barium, cobalt, nickel, manganese, iron, zinc, aluminium, indium or bismuth.
The mechanism that the present invention prepares sulfur doping Graphene is as follows:
In the mixed system of sulphur source and rich carbon organic salt or rich carbon organic acid and salt, rich carbon organic acid or rich carbon organic salt as carbon source in high temperature non-oxidizing atmosphere, through pyrolysis, the metal oxide surface that carbon atom is grown in position becomes nuclear rearrangement, rearrangement presents the growth of two-dimensional directional according to oxide surface template, and continuity is good, thereby obtain the mixture of porous graphene and metal oxide.Meanwhile, after the pyrolysis of sulphur source, produce active sulphur, participated in the rearrangement process of carbon atom, realize the growth of the in-situ doped Graphene of sulphur; And not only provide active sulphur for organosulfur compound, and part carbon is also provided, realize the growth of the in-situ doped Graphene of sulphur.Metal oxide has and is dissolved in sour feature, so mixture is after cleanup acid treatment, can obtain pure sulfur doping porous graphene.
From foregoing description, beneficial effect of the present invention is:
Due to the present invention only need by non-oxidizing atmosphere, heat sulphur source and organic salt or with the mixture of organic acid and salt, can prepare the mixture of sulfur doping Graphene and metal oxide, the follow-up metal oxide that can remove in mixture by conventional impurity removal process such as washing lotion washings obtains the sulfur doping Graphene that purity is higher, therefore compared to existing technologies, it is simple that the present invention has technique, with short production cycle, can be in-situ doped etc. advantage, and the sulfur doping Graphene preparing has porousness, the feature that specific surface area is large, can be widely used in lithium ion battery, ultracapacitor, lead-acid cell, water treatment, electrocatalysis, the every field such as photochemical catalysis.
Preferably, the weight ratio of described organic acid and salt is organic acid: salt=1: 9-9: 1.
Preferably, the weight ratio of described sulphur source and organic salt is sulphur source: organic salt=0.1: 100-1: 10.
Preferably, the weight ratio of the mixture of described sulphur source and organic acid and salt is sulphur source: mixture=0.1 of organic acid and salt: 100-1: 10.
Preferably, one or more in nitrogen, argon gas, hydrogen and ammonia of described non-oxidizing atmosphere form.
Preferably, due to sulfur doping Graphene at high temperature contact with air be easy to oxidized, the problems such as the product purity causing for fear of oxidation and Quality Down, during the metal oxide of the present invention in removing mixture, preferably in the following ways: under the condition of isolated air and/or mixture temperature adopt the mode of washing lotion washing to remove the metal oxide in mixture under lower than the condition of 100 ℃, described washing lotion is selected from one or more in hydrochloric acid, nitric acid, sulfuric acid, acetic acid and oxalic acid.Preferred, one or both in employing 37% concentrated hydrochloric acid and 30% acetic acid, pickling 4-8 hour under the temperature condition of 40-60 ℃.After having washed, further suction filtration is to being dried to obtain highly purified sulfur doping Graphene.
Preferably, the speed of described heating is 0.5-15 ℃/min.When heating rate is too fast, the productive rate of sulfur doping Graphene is lower, and excessively slow heating rate, can greatly extend again the production cycle of product.Preferred, the speed of described heating is 2-10 ℃/min.
Preferably, in order to improve the quality product of sulfur doping Graphene, described sulphur source and organic salt or under non-oxidizing atmosphere, be heated to 400-1600 ℃ with the mixture of organic acid and salt after be incubated 1-6h.
Experimental technique described in following embodiment, if no special instructions, is ordinary method; Described reagent and material, if no special instructions, all can obtain from commercial channels.
Embodiment 1, take 2 grams of citrate of lime and 0.2 gram of dodecyl thioether, put it in magnetic boat, then with tube furnace, in nitrogen, by the speed of 2 ℃/min, be warming up to 600 ℃, 600 ℃ of heating 2 hours, obtain sulfur doping Graphene and calcium oxide mixture, with 37% concentrated hydrochloric acid of 10 milliliters, at 50 ℃, wash 4 hours, suction filtration, to dry, obtains sulfur doping Graphene.Through ultimate analysis, the sulphur content of this sulfur doping Graphene is 5.1%.
Embodiment 2, take 2 grams of Zinc Gluconates and 0.5 gram of tetramethylene sulfone, put it in magnetic boat, then with tube furnace, in argon gas, by the speed of 2 ℃/min, be warming up to 600 ℃, 600 ℃ of heating 2 hours, obtain sulfur doping Graphene and zinc oxide mixture, with 37% concentrated hydrochloric acid of 10 milliliters, at 50 ℃, wash 4 hours, suction filtration, to dry, obtains sulfur doping Graphene.Through ultimate analysis, the sulphur content of this sulfur doping Graphene is 4.5%.
Embodiment 3, take 2 grams of Eighteen alkyl acid calcium and 0.9 gram of propylene sulfite, put it in magnetic boat, then with tube furnace, in nitrogen, by the speed of 10 ℃/min, be warming up to 600 ℃, 600 ℃ of heating 2 hours, obtain sulfur doping Graphene and calcium oxide mixture, with 30% acetic acid of 10 milliliters, at 50 ℃, wash 4 hours, suction filtration, to dry, obtains sulfur doping Graphene.Through ultimate analysis, the sulphur content of this sulfur doping Graphene is 4.1%.
Embodiment 4, take 1 gram of zinc oleate and 0.4 gram of ethylene sulfite, put it in magnetic boat, then with tube furnace, in argon gas and hydrogen mixed gas, by the speed of 5 ℃/min, be warming up to 800 ℃, 800 ℃ of heating 2 hours, obtain sulfur doping Graphene and zinc oxide mixture, with 37% concentrated hydrochloric acid of 10 milliliters, at 50 ℃, wash 4 hours, suction filtration, to dry, can obtain sulfur doping Graphene.Through ultimate analysis, the sulphur content of this sulfur doping Graphene is 3.5%.
Embodiment 5, take 1 gram of oleic acid, 1 gram of zinc acetate and 0.5 gram of ethylene sulfite, put it in magnetic boat, then with tube furnace, in nitrogen, by the speed of 5 ℃/min, be warming up to 800 ℃, 800 ℃ of heating 2 hours, obtain sulfur doping Graphene and zinc oxide mixture, with 37% concentrated hydrochloric acid of 10 milliliters, at 50 ℃, wash 4 hours, suction filtration, to dry, can obtain sulfur doping Graphene.Through ultimate analysis, the sulphur content of this sulfur doping Graphene is 2.7%.
Embodiment 6, take 2 grams of citrate of lime, 1 gram of calcium tartrate and 0.3 gram of dodecyl thioether, put it in magnetic boat, then with tube furnace, in nitrogen, by the speed of 2 ℃/min, be warming up to 900 ℃, 900 ℃ of heating 2 hours, obtain sulfur doping Graphene and calcium oxide mixture, with 37% concentrated hydrochloric acid of 10 milliliters, at 50 ℃, wash 4 hours, suction filtration, to dry, can obtain sulfur doping Graphene.Through ultimate analysis, the sulphur content of this sulfur doping Graphene is 3.6%.
Embodiment 7, take 2 grams of citrate of lime, 0.2 gram of dodecyl thioether and 0.1 gram of tetramethylene sulfone, put it in magnetic boat, then with tube furnace, in nitrogen, by the speed of 2 ℃/min, be warming up to 1000 ℃, 1000 ℃ of heating 2 hours, obtain sulfur doping Graphene and calcium oxide mixture, with 37% concentrated hydrochloric acid of 10 milliliters, at 50 ℃, wash 4 hours, suction filtration, to dry, can obtain sulfur doping Graphene.Through ultimate analysis, the sulphur content of this sulfur doping Graphene is 4.8%.
The sulfur doping Graphene that above-described embodiment 1-7 is prepared, carries out electron-microscope scanning, and the scanning electron microscope (SEM) photograph obtaining can be with reference to shown in Fig. 1.Known as shown in Figure 1, the sulfur doping Graphene that the present invention finally prepares is formed and is presented cell texture by flaky texture.
The foregoing is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or conversion of equivalent flow process that utilizes specification sheets of the present invention and accompanying drawing content to do; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (10)
1. a sulfur doping graphene preparation method, is characterized in that, comprising:
By sulphur source and organic salt or be heated to 300-1600 ℃ with the mixture of organic acid and salt under non-oxidizing atmosphere, obtain the mixture of sulfur doping Graphene and metal oxide;
Remove the metal oxide in mixture, obtain sulfur doping Graphene;
Wherein, described sulphur source is selected from one or more in di-n-octyl thioether, dodecyl thioether, tetramethylene sulfone, 4-propylthio vinyl acetate, sulfuric acid vinyl ester, propylene sulfite, sulfuric acid propylene, 4-methyl ethylene sulfite and butylene sulfite;
Wherein, described organic salt is selected from alkyl soap that Citrate trianion, gluconate, tartrate, D-VB5 salt, threose acid salt, the carbonatoms of magnesium, calcium, strontium, barium, cobalt, nickel, manganese, iron, zinc, aluminium, indium or bismuth are 8-24 and one or more in oleate;
Wherein, described organic acid is selected from citric acid, gluconic acid, tartrate, D-VB5, threonic acid, alkyl lipid acid that carbonatoms is 8-24 and one or more in oleic acid;
Wherein, described salt is selected from one or more in acetate, nitrate, chlorate, Bromide and the iodized salt of magnesium, calcium, strontium, barium, cobalt, nickel, manganese, iron, zinc, aluminium, indium or bismuth.
2. sulfur doping graphene preparation method according to claim 1, is characterized in that: described sulphur source and organic salt or under non-oxidizing atmosphere, be heated to 400-1600 ℃ with the mixture of organic acid and salt after be incubated 1-6h.
3. sulfur doping graphene preparation method according to claim 1, it is characterized in that: under the condition of isolated air and/or mixture temperature adopt the mode of washing lotion washing to remove the metal oxide in mixture under lower than the condition of 100 ℃, described washing lotion is selected from one or more in hydrochloric acid, nitric acid, acetic acid and oxalic acid.
4. sulfur doping graphene preparation method according to claim 1, is characterized in that: one or more in nitrogen, argon gas, hydrogen and ammonia of described non-oxidizing atmosphere form.
5. sulfur doping graphene preparation method according to claim 1, is characterized in that: the speed of described heating is 0.5-15 ℃/min.
6. sulfur doping graphene preparation method according to claim 5, is characterized in that: the speed of described heating is 2-10 ℃/min.
7. sulfur doping graphene preparation method according to claim 1, is characterized in that: the weight ratio of described organic acid and salt is organic acid: salt=1: 9-9: 1.
8. sulfur doping graphene preparation method according to claim 1, is characterized in that: the weight ratio of described sulphur source and organic salt is sulphur source: organic salt=0.1: 100-1: 10.
9. sulfur doping graphene preparation method according to claim 1, is characterized in that: the weight ratio of the mixture of described sulphur source and organic acid and salt is sulphur source: mixture=0.1 of organic acid and salt: 100-1: 10.
10. the sulfur doping Graphene being prepared by the preparation method described in claim 1 to 9 any one.
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| CN105731428A (en) * | 2014-12-12 | 2016-07-06 | 中国科学院过程工程研究所 | Preparation method and application of sulfur-doped graphene and derivatives thereof |
| CN107221652A (en) * | 2017-03-28 | 2017-09-29 | 深圳新宙邦科技股份有限公司 | A kind of sulfur doping carbon material and preparation method thereof |
| CN107973289A (en) * | 2017-11-08 | 2018-05-01 | 华侨大学 | A kind of sulfur doping graphene catalysis material and preparation method thereof |
| CN111547705A (en) * | 2020-05-12 | 2020-08-18 | 中国计量大学 | Preparation method of porous carbon electrode material |
| JP2020142960A (en) * | 2019-03-06 | 2020-09-10 | 株式会社クラレ | Porous carbon and method for producing porous carbon |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105731428A (en) * | 2014-12-12 | 2016-07-06 | 中国科学院过程工程研究所 | Preparation method and application of sulfur-doped graphene and derivatives thereof |
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| CN107221652A (en) * | 2017-03-28 | 2017-09-29 | 深圳新宙邦科技股份有限公司 | A kind of sulfur doping carbon material and preparation method thereof |
| CN107973289A (en) * | 2017-11-08 | 2018-05-01 | 华侨大学 | A kind of sulfur doping graphene catalysis material and preparation method thereof |
| JP2020142960A (en) * | 2019-03-06 | 2020-09-10 | 株式会社クラレ | Porous carbon and method for producing porous carbon |
| JP7338993B2 (en) | 2019-03-06 | 2023-09-05 | 株式会社クラレ | Porous carbon and method for producing porous carbon |
| CN111547705A (en) * | 2020-05-12 | 2020-08-18 | 中国计量大学 | Preparation method of porous carbon electrode material |
| CN111547705B (en) * | 2020-05-12 | 2022-03-29 | 中国计量大学 | Preparation method of porous carbon electrode material |
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Effective date of registration: 20191216 Address after: 518000 5th floor, Wanke yunchuang, block B, Bolton Science Park, intersection of Chuangke road and chaguang Road, Xili street, Nanshan District, Shenzhen City, Guangdong Province Patentee after: Shenzhen Yixin technology R & D Co., Ltd Address before: 518000 Guangdong province Shenzhen City Pingshan Pingshan sand Tang with rich industrial area Patentee before: Shenzhen Xinyubang Science and Technology Co., Ltd. |