CN104140097A - Phosphor doped grapheme and preparing method thereof - Google Patents
Phosphor doped grapheme and preparing method thereof Download PDFInfo
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Abstract
The invention relates to phosphor doped grapheme and a preparing method of the phosphor doped grapheme. The preparing method includes the steps that a mixture of a phosphorus source, an organic salt or organic acid and salt is heated to 300 DEG C-1600 DEG C in a non-oxidizing atmosphere to obtain a mixture of the phosphor doped grapheme and a metal oxide, and the metal oxide in the mixture is removed to obtain the phosphor doped grapheme. According to the preparing method, the mixture of the phosphorus source, the organic salt or the organic acid and the salt is heated in the non-oxidizing atmosphere, the concepts of carbonizing the grapheme through the organic salt, nucleating inorganic oxide and generating active phosphorus through phosphorus source pyrolysis are used for preparing the phosphor doped grapheme. The method has the advantages that the technology is simple, the production cycle is short, and in-situ doping is allowed, the prepared phosphor doped grapheme has the advantages of being porous, large in specific area and free of agglomeration and can be widely applied to various fields of lithium ion batteries, supercapacitors, lead-acid batteries, water treatment, electro-catalyses, photocatalyses and the like.
Description
Technical field
The present invention relates to carbon material technical field, is a kind of phosphorus doping Graphene and preparation method thereof specifically.
Background technology
Along with the exhaustion of petroleum resources, clean energy technology receives people's concern day by day.Lithium ion battery, ultracapacitor, fuel cell equal energy source transform and storage art has noticeable application potential.Advanced electrode materials and catalyzer are core and the development bottleneck of this class energy device.In recent years, with the development of Graphene and energy device technology, Heteroatom doping Graphene becomes the study hotspot in these fields.
Fewer about the report of phosphorus doping Graphene in prior art.The people such as Hou Yanglong are by graphene oxide mixing triphenyl phosphorus through Overheating Treatment, and the phosphorus content obtaining in the Graphene of phosphorus doping is 1.81% (Advanced Materials, 201,25,4932-4937).In Chinese patent CN 103495430 A, by mixed oxidization graphite and phosphorous ionic liquid, obtain doped graphene through Overheating Treatment.In above-mentioned technology, all need to, taking graphene oxide as substrate, can not original position prepare phosphorus doping Graphene, and relate to multiple experimental procedures, complex process, inefficiency.
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, phosphorus doping graphene preparation method that can in-situ doped phosphorus.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is:
A kind of phosphorus doping graphene preparation method, comprising:
By phosphorus source and organic salt or be heated to 300-1600 DEG C with the mixture of organic acid and salt under non-oxidizing atmosphere, obtain the mixture of phosphorus doping Graphene and metal oxide;
Remove the metal oxide in mixture, obtain phosphorus doping Graphene;
Wherein, described phosphorus source is selected from one or more in elemental phosphorous, phosphoric acid salt, phosphate compounds and phosphite ester compound;
Wherein, described organic salt is selected from one or more in alkyl soap and the oleate 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;
Wherein, described organic acid is selected from one or more in alkyl lipid acid and the oleic acid that citric acid, gluconic acid, tartrate, D-VB5, threonic acid, carbonatoms are 8-24;
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 phosphorus, the phosphorus 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.
Brief description of the drawings
Figure 1 shows that the scanning electron microscope (SEM) photograph of phosphorus doping Graphene prepared by the embodiment of the present invention 1.
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 heat phosphorus source and organic salt or the mixture with organic acid and salt in non-oxidizing atmosphere; utilize organic salt carbonized graphite alkene, inorganic oxide nucleation and the pyrolysis of phosphorus source to produce the theory of active phosphorus; prepare the original position phosphorus 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 phosphorus doping Graphene preparing can be applicable to the every field such as lithium ion battery, ultracapacitor, lead-acid cell, water treatment, electrocatalysis, photochemical catalysis.
Phosphorus doping graphene preparation method provided by the invention, comprising:
By phosphorus source and organic salt or be heated to 300-1600 DEG C with the mixture of organic acid and salt under non-oxidizing atmosphere, obtain the mixture of phosphorus doping Graphene and metal oxide;
Remove the metal oxide in mixture, obtain phosphorus doping Graphene;
Wherein, described phosphorus source is selected from one or more in elemental phosphorous, phosphoric acid salt, phosphate compounds and phosphite ester compound;
Wherein, described organic salt is selected from one or more in alkyl soap and the oleate 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;
Wherein, described organic acid is selected from one or more in alkyl lipid acid and the oleic acid that citric acid, gluconic acid, tartrate, D-VB5, threonic acid, carbonatoms are 8-24;
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 phosphorus doping Graphene is as follows:
In the mixed system of phosphorus 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, reset the growth that presents 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 phosphorus source, produce active phosphorus, participated in the rearrangement process of carbon atom, realize the growth of the in-situ doped Graphene of phosphorus; And not only provide active phosphorus for organo phosphorous compounds, and part carbon is also provided, realize the growth of the in-situ doped Graphene of phosphorus.Metal oxide has the sour feature that is dissolved in, and therefore mixture, after cleanup acid treatment, can obtain pure phosphorus doping porous graphene.
From foregoing description, beneficial effect of the present invention is:
Because the present invention only needs by heat phosphorus source and organic salt or the mixture with organic acid and salt in non-oxidizing atmosphere, can prepare the mixture of phosphorus 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 phosphorus 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 phosphorus 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, described phosphorus source is selected from one or more in red phosphorus, Secondary ammonium phosphate, primary ammonium phosphate, phosphoric acid, phosphorous acid, trimethyl phosphite 99, triethyl phosphate, tributyl phosphate, trioctyl phosphate, triphenylphosphate, trimethyl phosphite, triethyl-phosphite, tributyl phosphate, tricresyl phosphite monooctyl ester and triphenyl phosphite.
Preferably, the weight ratio of described organic acid and salt is 1: 9-9: 1.
Preferably, the weight ratio of described phosphorus source and organic salt is 0.1: 100-1: 10.
Preferably, the weight ratio of the mixture of described phosphorus source and organic acid and salt is 0.1: 100-1: 10.
Preferably, described non-oxidizing atmosphere is made up of one or more in nitrogen, argon gas, hydrogen and ammonia.
Preferably, due to phosphorus doping Graphene at high temperature contact with air be easy to oxidized, the problem such as product purity and Quality Down causing for fear of oxidation, the present invention is in the time of the metal oxide of removing in 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 DEG C, described washing lotion is selected from one or more in hydrochloric acid, nitric 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 DEG C.After having washed, further suction filtration is to being dried to obtain highly purified phosphorus doping Graphene.
Preferably, the speed of described heating is 0.5-15 DEG C/min.In the time that heating rate is too fast, the productive rate of phosphorus 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 DEG C/min.
Preferably, in order to improve the quality product of phosphorus doping Graphene, described phosphorus source and organic salt or under non-oxidizing atmosphere, be heated to 350-1600 DEG C 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 5.55 grams of calcium stearates and 0.45 gram of triphenylphosphate, put it in magnetic boat, then in argon gas, be warming up to 700 DEG C by the speed of 4 DEG C/min with tube furnace, 700 DEG C of heating 2 hours, obtain phosphorus doping Graphene and calcium oxide mixture,, at 50 DEG C, wash 4 hours with 37% concentrated hydrochloric acid of 10 milliliters, suction filtration, to dry, can obtain phosphorus doping Graphene.Through ultimate analysis, the phosphorus content of this phosphorus doping Graphene is 6.1%.
Embodiment 2, take 2 grams of citrate of lime and 0.2 gram of trioctyl phosphate, put it in magnetic boat, then in nitrogen, be warming up to 600 DEG C by the speed of 2 DEG C/min with tube furnace, 600 DEG C of heating 2 hours, obtain phosphorus doping Graphene and calcium oxide mixture,, at 50 DEG C, wash 4 hours with 37% concentrated hydrochloric acid of 10 milliliters, suction filtration, to dry, can obtain phosphorus doping Graphene.Through ultimate analysis, the phosphorus content of this phosphorus doping Graphene is 4.2%.
Embodiment 3, take 2 grams of Eighteen alkyl acid calcium and 0.9 gram of triphenyl phosphite, put it in magnetic boat, then in nitrogen, be warming up to 600 DEG C by the speed of 10 DEG C/min with tube furnace, 600 DEG C of heating 2 hours, obtain phosphorus doping Graphene and calcium oxide mixture,, at 50 DEG C, wash 4 hours with 30% acetic acid of 10 milliliters, suction filtration, to dry, can obtain phosphorus doping Graphene.Through ultimate analysis, the phosphorus content of this phosphorus doping Graphene is 6.4%.
Embodiment 4, take 1 gram of zinc oleate and 0.4 gram of tricresyl phosphite monooctyl ester, put it in magnetic boat, then in argon gas and hydrogen mixed gas, be warming up to 800 DEG C by the speed of 5 DEG C/min with tube furnace, 800 DEG C of heating 2 hours, obtain phosphorus doping Graphene and zinc oxide mixture,, at 50 DEG C, wash 4 hours with 37% concentrated hydrochloric acid of 10 milliliters, suction filtration, to dry, can obtain phosphorus doping Graphene.Through ultimate analysis, the phosphorus content of this phosphorus doping Graphene is 5.6%.
Embodiment 5, take 1 gram of oleic acid, 1 gram of zinc acetate and 0.5 gram of tributyl phosphate, put it in magnetic boat, then in nitrogen, be warming up to 800 DEG C by the speed of 5 DEG C/min with tube furnace, 800 DEG C of heating 2 hours, obtain phosphorus doping Graphene and zinc oxide mixture,, at 50 DEG C, wash 4 hours with 29% strong aqua of 10 milliliters, suction filtration, to dry, can obtain phosphorus doping Graphene.Through ultimate analysis, the phosphorus content of this phosphorus doping Graphene is 5.9%.
Embodiment 6, take 1 gram of gluconic acid, 1 gram of calcium acetate and 0.6 gram of triphenyl phosphite, put it in magnetic boat, then in nitrogen, be warming up to 400 DEG C by the speed of 5 DEG C/min with tube furnace, 400 DEG C of heating 6 hours, obtain phosphorus doping Graphene and zinc oxide mixture,, at 50 DEG C, wash 4 hours with 37% concentrated hydrochloric acid of 10 milliliters, suction filtration, to dry, can obtain phosphorus doping Graphene.Through ultimate analysis, the phosphorus content of this phosphorus doping Graphene is 5.5%.
Embodiment 7, take 2 grams of manganese citrates and 0.6 gram of trimethyl phosphite, put it in magnetic boat, then in nitrogen, be warming up to 1200 DEG C by the speed of 5 DEG C/min with tube furnace, 1200 DEG C of heating 2 hours, obtain phosphorus doping Graphene and manganese monoxide mixture,, at 50 DEG C, wash 4 hours with 30% the acetic acid of 10 milliliters, suction filtration, to dry, can obtain phosphorus doping Graphene.Through ultimate analysis, the phosphorus content of this phosphorus doping Graphene is 6.35%.
Embodiment 8, take 2 grams of citrate of lime, 3 grams of calcium stearates and 0.25 gram of trioctyl phosphate, put it in magnetic boat, then in nitrogen, be warming up to 850 DEG C by the speed of 2 DEG C/min with tube furnace, 850 DEG C of heating 4 hours, obtain phosphorus doping Graphene and calcium oxide mixture,, at 50 DEG C, wash 4 hours with 37% concentrated hydrochloric acid of 10 milliliters, suction filtration, to dry, can obtain phosphorus doping Graphene.Through ultimate analysis, the phosphorus content of this phosphorus doping Graphene is 4.3%.
Embodiment 9, take 2 grams of citrate of lime, 3 grams of calcium stearates and 0.2 gram of primary ammonium phosphate, put it in magnetic boat, then in nitrogen, be warming up to 900 DEG C by the speed of 2 DEG C/min with tube furnace, 900 DEG C of heating 2 hours, obtain phosphorus doping Graphene and calcium oxide mixture,, at 50 DEG C, wash 4 hours with 37% concentrated hydrochloric acid of 10 milliliters, suction filtration, to dry, can obtain phosphorus doping Graphene.Through ultimate analysis, the phosphorus content of this phosphorus doping Graphene is 4.2%.
Embodiment 10, take 4 grams of calcium stearates and 0.3 gram of Secondary ammonium phosphate, put it in magnetic boat, then in nitrogen, be warming up to 600 DEG C by the speed of 2 DEG C/min with tube furnace, 600 DEG C of heating 2 hours, obtain phosphorus doping Graphene and calcium oxide mixture,, at 50 DEG C, wash 4 hours with 37% concentrated hydrochloric acid of 10 milliliters, suction filtration, to dry, can obtain phosphorus doping Graphene.Through ultimate analysis, the phosphorus content of this phosphorus doping Graphene is 4.1%.
Embodiment 11, take 4 grams of oleic acid, 4 grams of manganous acetates and 0.3 gram of red phosphorus, put it in magnetic boat, then in nitrogen, be warming up to 600 DEG C by the speed of 2 DEG C/min with tube furnace, 600 DEG C of heating 2 hours, obtain phosphorus doping Graphene and manganese monoxide mixture,, at 50 DEG C, wash 4 hours with 37% concentrated hydrochloric acid of 10 milliliters, suction filtration, to dry, can obtain phosphorus doping Graphene.Through ultimate analysis, the phosphorus content of this phosphorus doping Graphene is 0.8%.
Embodiment 12, take 4 grams of stearic acid, 0.4 gram of zinc nitrate and 0.3 gram of Secondary ammonium phosphate, put it in magnetic boat, then in nitrogen, be warming up to 600 DEG C by the speed of 2 DEG C/min with tube furnace, 600 DEG C of heating 2 hours, obtain phosphorus doping Graphene and calcium oxide mixture,, at 50 DEG C, wash 4 hours with 37% concentrated hydrochloric acid of 10 milliliters, suction filtration, to dry, can obtain phosphorus doping Graphene.Through ultimate analysis, the phosphorus content of this phosphorus doping Graphene is 4.5%.
Embodiment 13, take 0.4 gram of oleic acid, 4 grams of barium iodides and 0.1 gram of Secondary ammonium phosphate, put it in magnetic boat, then in nitrogen, be warming up to 600 DEG C by the speed of 2 DEG C/min with tube furnace, 600 DEG C of heating 2 hours, obtain phosphorus doping Graphene and calcium oxide mixture,, at 50 DEG C, wash 4 hours with 37% concentrated hydrochloric acid of 10 milliliters, suction filtration, to dry, can obtain phosphorus doping Graphene.Through ultimate analysis, the phosphorus content of this phosphorus doping Graphene is 6.0%.
The phosphorus doping Graphene that above-described embodiment 1-13 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 phosphorus doping Graphene that the present invention finally prepares presents cell 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 phosphorus doping graphene preparation method, is characterized in that, comprising:
By phosphorus source and organic salt or be heated to 300-1600 DEG C with the mixture of organic acid and salt under non-oxidizing atmosphere, obtain the mixture of phosphorus doping Graphene and metal oxide;
Remove the metal oxide in mixture, obtain phosphorus doping Graphene;
Wherein, described phosphorus source is selected from one or more in elemental phosphorous, phosphoric acid salt, phosphate compounds and phosphite ester compound;
Wherein, described organic salt is selected from one or more in alkyl soap and the oleate 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;
Wherein, described organic acid is selected from one or more in alkyl lipid acid and the oleic acid that citric acid, gluconic acid, tartrate, D-VB5, threonic acid, carbonatoms are 8-24;
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. phosphorus doping graphene preparation method according to claim 1, is characterized in that: described phosphorus source is selected from one or more in red phosphorus, Secondary ammonium phosphate, primary ammonium phosphate, phosphoric acid, phosphorous acid, trimethyl phosphite 99, triethyl phosphate, tributyl phosphate, trioctyl phosphate, triphenylphosphate, trimethyl phosphite, triethyl-phosphite, tributyl phosphate, tricresyl phosphite monooctyl ester and triphenyl phosphite.
3. phosphorus doping graphene preparation method according to claim 1, is characterized in that: described phosphorus source and organic salt or under non-oxidizing atmosphere, be heated to 350-1600 DEG C with the mixture of organic acid and salt after be incubated 1-6h.
4. phosphorus 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 DEG C, described washing lotion is selected from one or more in hydrochloric acid, nitric acid, acetic acid and oxalic acid.
5. phosphorus doping graphene preparation method according to claim 1, is characterized in that: described non-oxidizing atmosphere is made up of one or more in nitrogen, argon gas, hydrogen and ammonia.
6. phosphorus doping graphene preparation method according to claim 1, is characterized in that: the speed of described heating is 0.5-15 DEG C/min.
7. phosphorus doping graphene preparation method according to claim 1, is characterized in that: the weight ratio of described organic acid and salt is 1: 9-9: 1.
8. phosphorus doping graphene preparation method according to claim 1, is characterized in that: the weight ratio of described phosphorus source and organic salt is 0.1: 100-1: 10.
9. phosphorus doping graphene preparation method according to claim 1, is characterized in that: the weight ratio of the mixture of described phosphorus source and organic acid and salt is 0.1: 100-1: 10.
10. the phosphorus doping Graphene being prepared by the preparation method described in claim 1 to 9 any one.
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| CN104817079A (en) * | 2015-05-07 | 2015-08-05 | 常州大学 | Preparation method of two-dimension phosphorus-doped graphene |
| CN104860291A (en) * | 2015-05-07 | 2015-08-26 | 常州大学 | Preparation method of phosphorus doped graphene sheet |
| CN105161691A (en) * | 2015-10-10 | 2015-12-16 | 岭南师范学院 | Preparation method of less-layer MoS2/phosphorus-doped graphene electrochemical sodium-storage combined electrode |
| CN107623118A (en) * | 2017-09-30 | 2018-01-23 | 三峡大学 | A kind of preparation method for the porous carbon negative pole material of phosphorus doping that coulombic efficiency first improves |
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| CN108658060A (en) * | 2018-06-26 | 2018-10-16 | 北京理工大学 | A kind of preparation method of the graphene nanometer sheet of the adjustable single layer phosphorus doping of band gap |
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| CN109772394A (en) * | 2019-01-16 | 2019-05-21 | 盐城工学院 | Phosphorus doping carbon/cuprous oxide composite catalyst and its preparation method and application |
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| 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 |
| CN113582165A (en) * | 2021-07-21 | 2021-11-02 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of phosphorus atom doped graphene nanocomposite |
| CN115636409A (en) * | 2022-10-20 | 2023-01-24 | 海城申合科技有限公司 | Method for preparing lithium ion carbon negative electrode material by organic phosphorus modified graphene oxide surface method |
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