CN107892291A - A kind of method that grapheme material is prepared using discarded object coconut husk as raw material - Google Patents
A kind of method that grapheme material is prepared using discarded object coconut husk as raw material Download PDFInfo
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- CN107892291A CN107892291A CN201710936104.7A CN201710936104A CN107892291A CN 107892291 A CN107892291 A CN 107892291A CN 201710936104 A CN201710936104 A CN 201710936104A CN 107892291 A CN107892291 A CN 107892291A
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Abstract
The invention discloses a kind of method that grapheme material is prepared using discarded object coconut husk as raw material.This method first crushes dried discarded object coconut husk；In N2Under atmospheric condition, it is placed in tube furnace；450~800 DEG C are warming up to, is incubated 1~2 hour；Continue to be warming up to 800~1000 DEG C, be incubated 1~2 hour, be slowly dropped to 25~35 DEG C, obtain pre- carbonized product；The pre- carbonized product of gained and Xiao Suan Xin ﹑ zinc chloride and potassium hydroxide are used alone or as a mixture, in N2Under atmospheric condition, it is placed in tube furnace；800~900 DEG C are warming up to, is incubated 1~2 hour；Continue to be warming up to 900~1200 DEG C, be incubated 0.5~2 hour, be slowly dropped to room temperature；The present invention's prepares graphene, and each peak of D, G and 2D is unimodal in Raman collection of illustrative plates, and IG/I2D is 1.25~2.31；The inventive method is simple, safety and environmental protection；Avoid to use in the redox method of graphite powder and largely use the concentrated sulfuric acid.
Description
Technical field
The present invention relates to biomass graphene, more particularly to a kind of side that graphene is prepared using discarded object coconut husk as raw material
Method, belong to biomass field of preparation of graphene.
Background technology
Discarded object coconut husk active carbon with high specific surface area has good adsorption performance, function as a kind of new Carbon Materials
Be widely used with added value it is high the characteristics of, there is high absorption capacity and large storage capacity compared with normal activated carbon, thus can apply
In gas separation, battery electrode and energy storage material, [Wang Guodong, Deng Xianlun, Zhu Guang are true etc., and KOH activation high-specific surface area coconut husks are lived
Property charcoal preparation and its property research, chemistry of forest product and industry, the 2nd phase of volume 33,108-112 in 2013].
Cocoanut active charcoal outward appearance is black, in broken shape, have hole is flourishing, absorption property is good, intensity is high, easy regeneration,
The advantages that economy and durability, it is a kind of to apply very extensive porous adsorbing material, especially CO2Good [the Jie of the absorption property of gas
Yang, Limin Yue, and Liping Guo etc., Efficient CO2Capture by Porous Carbons
Derived from Coconut Shell, Energy Fuels 2017,31,4287-4293].Porous material is utilized into chemistry
Material carries out the modification of surface and pore structure, improves performance of the adsorbent, prepares super capacitor, its excellent performance [Juan Mi,
Xiao-Rong Wang, and Wen-Cui Li, Coconut-Shell-Based Porous Carbons with a
Tunable Micro/Mesopore Ratio for High-Performance Supercapa, Energy Fuels
2012,26,5321-5329]。
Activated coco nut charcoal is widely used in the various aspects of industrial and agricultural production, and the alkali-free sweetening such as petrochemical industry is (refined
Removal of mercaptans), ethene desalted water (refining filler), catalyst carrier (palladium, platinum, rhodium etc.), Water warfare and sewage disposal；Power industry
Power plant's water treatment and protection；The chemical catalyst and carrier of chemical industry, gas purification, solvent recovery and grease etc. it is de-
Color, refine；The beverage of food service industry, drinks, sodium glutamate mother liquid and food it is refined, decolourize；The gold extraction of gold industry, tail washings
Recovery；The sewage disposal of environmental protection industry (epi), the improvement of waste gas and pernicious gas, gas purification；And relevant industries cigaratte filter,
Timber floor is moistureproof, inhales taste, automobile gasoline evaporative emission control, the preparation of various impregnating agent liquid etc..
The method that prior art not yet hair prepares graphene using discarded object coconut husk as raw material, while prior art industrializes
During producing graphene, usually using graphite powder as raw material, obtained with oxidation-reduction method, this production technology will use dense sulphur
Acid, production cost is high, big for environment pollution.
The content of the invention
The object of the present invention is to overcome the problems of the prior art, there is provided a kind of high efficiency, cost is low, safety and environmental protection
The method using discarded cocoanut shell for raw material preparation biomass graphene, gained biomass graphene is multi-layer graphene.
Coconut husk derives from natural biomass, is the endocarp of babassu coconut, containing lignin 36.51%, fiber
Element 53.06%, pentosan 29.27%, quality is hard.Coconut husk yield in the whole world is about 8000t or so at present, and coconut husk is arbitrarily lost
Abandon, not only pollution of ecological environment, endanger human health, and occupy the land resource of preciousness, therefore, strengthen to coconut husk resource
Comprehensive utilization tool be of great significance.
Useless coconut husk coconut husks in addition to being commonly used to the fields such as handicraft, composite reinforcing material, furniture, weaving, food are made
For agriculture and forestry organic waste material, it has the characteristics that, and special institutional framework, compactness are high, ash content is low, high mechanical strength, are advantageous to micropore
The generation of structure, it is the quality raw materials for preparing activated carbon.Processing for various waste water and waste gas, it is also possible to make excellent carrier
Catalyst-loaded catalytic degradation organic wastewater and waste gas and catalyze and synthesize organic compound [Jiang Baiquan, Zeng Fang, once celebrate virtue etc.,
The preparation of cocoanut active charcoal and absorption Acid Brilliant Scarlet GR dyestuff dynamics, Treatment of Industrial Water 2014-06,34 (6), 17-19].But
The method that discarded object coconut husk is prepared as to biomass graphene has no report.
The purpose of the present invention is achieved through the following technical solutions：
A kind of method that grapheme material is prepared using discarded object coconut husk as raw material, comprises the following steps：
1) dried discarded object coconut husk is crushed, obtains discarded object coconut shell powder；
2) by discarded object coconut shell powder obtained by step 1), in N2Under atmospheric condition, it is small to be warming up to 450-800 DEG C of insulation 1~2
When；Continue to be warming up to 800~1000 DEG C, be incubated 0.5~2 hour, be slowly dropped to 25~35 DEG C, obtain the pre- carbonized product of coconut husk；
3) pre- carbonized product obtained by step 2) is mixed with reaction raw materials, the weight ratio of pre- carbonized product and reaction raw materials is
1：1~5, in N2Under atmospheric condition, it is warming up to 800~900 DEG C and is incubated 1~2 hour；Continue to be warming up to 900~1200 DEG C, insulation
0.5~2 hour, room temperature is slowly dropped to, obtains discarded object coconut husk biomass graphene；The reaction raw materials are Lvization Xin ﹑ nitric acid
One or more in zinc and potassium hydroxide.
Further to realize the object of the invention, it is preferable that it is described be warming up to 450-800 DEG C control programming rate for 0.5~
2.0 DEG C/min.
Preferably, described to continue to be warming up to 900~1200 DEG C, it is 3.0~5.0 DEG C/min to control programming rate.
Preferably, step 2) is described is slowly dropped to be slowly dropped to room temperature control cooling rate described in 25~35 DEG C and step 3)
For 3~5 DEG C/min.
Preferably, the discarded object coconut husk of the drying is will to be left discarded coconut husk after edible coconut to pass through 95~120 DEG C
Toast obtained by 12-24 hours.
Preferably, described cool to after room temperature of step 3) also includes taking out sample, and eluant, eluent, cleaning are used as by the use of deionized water
For neutrality, washed repeatedly with absolute ethyl alcohol, 100-120 DEG C of drying.
Preferably, the specific surface area of discarded object coconut husk biomass graphene obtained by step 3) is 1170~2673m2/g。
Preferably, the D ﹑ G and 2D peaks of the Raman spectrum of discarded object coconut husk biomass graphene obtained by step 3) are unimodal；
And IG/I2D is 1.25~2.31.
Preferably, step 1) also includes sieving after obtaining discarded object coconut shell powder；The sieving was 50~100 mesh sieves.
Preferably, step 2), which is warming up to 450-800 DEG C and is incubated 1~2 hour, is carried out in tube furnace；Step 3) is warming up to
800~900 DEG C, which are incubated 1~2 hour, is carried out in tube furnace.
Compared with prior art, the present invention has the advantage that：
(1) discarded object coconut husk is organic waste, pollutes environment, will there is substantial amounts of discarded object coconut husk every year；Present invention side
Method is avoided using needing to use the substantial amounts of concentrated sulfuric acid in oxidation-reduction method so that a large amount of discharge of wastewater, Wu contaminate Huan Jing ﹑ in industry
Danger and the increase production cost of blast are avoided under the conditions of metaplasia production；
(2) the discarded object coconut husk biomass graphene for preparing of the present invention, IG/I2D are 1.25~2.31, and 2D is into list
Peak, show that [Li Jia, Shi Fenghui, Lv Jing etc., arc process prepares graphene to discarded object coconut husk biomass graphene for multi-layer graphene
The sign of material and evaluation, composite journal, 2015,32 (6)：1658-1622]；Life is improved under commercial production conditions
Material quality of graphene, quality assurance is provided for downstream product (conductive carbon pastes, graphene battery, lightweight bulletproof clothing etc.)；
(3) discarded object coconut husk biomass graphene prepared by the present invention, specific surface area is (1170~2673m2/ g), this with
Graphene specific surface area (the 2620m of theoretical prediction2/ g) it is close, further prove discarded object coconut husk biomass produced by the present invention
Graphene, ensure the quality of graphene, discarded object coconut husk can be made to turn into biomass graphene, turn into the useful electronics of electronics industry
Material.
(4) relative to this reducing process of prior art, invent and continuous industrial production can be achieved, have significant technique excellent
Gesture.
Brief description of the drawings
Fig. 1 is the Raman collection of illustrative plates of the products therefrom of embodiment 1.
Embodiment
To more fully understand the present invention, this present invention is described further with reference to embodiment, but the present invention
Embodiment is unlimited so.
Embodiment 1
A kind of method that grapheme material is prepared using discarded object coconut husk as raw material, comprises the following steps：
It will be cleaned from market of farm produce discarded object coconut husk, 95 DEG C of drying overnight, then, crushed 50 mesh sieves, be discarded
Thing coconut shell powder；In N2Under atmospheric condition, discarded object coconut shell powder is placed in tube furnace.It is 1.0 DEG C/minute to control programming rate
Clock is incubated 2 hours to 450 DEG C；Continue to heat up, it is 5.0 DEG C/min to control programming rate, is warming up to 800 DEG C, is incubated 1 hour,
Cooling rate control is 5 DEG C/min, slowly cools to room temperature, obtains the pre- carbonized product of discarded object coconut husk；
Weigh the pre- carbonized product of 2 grams of discarded object coconut husks and 4 grams of potassium hydroxide and the mixing of 1 gram of zinc nitrate, then add go from
Sub- water 1mL dissolvings.Stirring, 80 DEG C of dryings, removes water, residue is in N2Under atmospheric condition, it is placed in tube furnace.Control rises
Warm speed is 1.0 DEG C/min, is warming up to 900 DEG C, is incubated 2 hours；Continue to heat up, it is 3.0 DEG C/min to control programming rate, is risen
Temperature is incubated 0.5 hour to 1100 DEG C, cools to room temperature, and cooling rate control is 5 DEG C/min, and room temperature takes out sample, uses watery hydrochloric acid
Wash, deionized water is as cleaning solution, until cleaning fluid is neutrality, wash 3 times with absolute ethyl alcohol, is dried at 60 DEG C.After tested, institute
Obtaining product specific surface area is：1957m2/g；Raman collection of illustrative plates is shown in accompanying drawing [instrument title as shown in Figure 1：Micro-Raman spectroscopy, type
Number：LabRAM Aramis manufacturers：French H.J.Y companies], Fig. 1 is a complete collection of illustrative plates of Raman, and D, G and 2D are list
Peak, meet the sign of graphite Raman collection of illustrative plates.Raman collection of illustrative plates shows that IG/I2D is 2.31 (with import U.S. graphene product
Quite).
It can be seen from figure 1 that in the present embodiment, in Fig. 1,2D peaks are unimodal, and discarded object coconut husk is multi-layer graphene, relative to
The graphene that graphite powder is prepared for raw material, simple production process, safety and environmental protection；The matter of downstream product can be above ensure that in application
Amount.
Embodiment 2
The discarded object coconut husk obtained from the market of farm produce is cleaned, and 110 DEG C of drying overnight, then, crushed 100 mesh sieves, obtain
Discarded object coconut shell powder；In N2Under atmospheric condition, discarded object coconut shell powder is placed in tube furnace.It is 0.5 to control programming rate
DEG C/min, 500 DEG C are warming up to, is incubated 2 hours；Continue to heat up, it is 5.0 DEG C/min to control programming rate, is warming up to 1000 DEG C,
Insulation 1 hour, room temperature is slowly cooled to, cooling rate control is 5 DEG C/min, obtains the pre- carbonized product of discarded object coconut husk；
Weigh the pre- carbonized product of 2 grams of discarded object coconut husks and 2 grams of potassium hydroxide and the mixing of 2 grams of zinc nitrates, then add go from
Sub- water 2mL dissolvings.Stirring, 90 DEG C of dryings, removes water, residue is in N2Under atmospheric condition, it is placed in tube furnace.Control rises
Warm speed is 0.5 DEG C/min, is warming up to 800 DEG C, is incubated 1 hour；Continue to heat up, it is 3.0 DEG C/min to control programming rate, is risen
Temperature is incubated 1 hour to 1100 DEG C, slowly cools to room temperature, and cooling rate control is 5 DEG C/min, and room temperature takes out sample, and use is dilute
Hydrochloric acid and deionized water are as eluant, eluent, until cleaning fluid is neutrality, wash 3 times with absolute ethyl alcohol, are dried at 60 DEG C.Through surveying
Examination, products therefrom specific surface area are：1990m2/ g, is determined with micro-Raman spectroscopy, LabRAM Aramis productions, France
H.J.Y companies.Raman collection of illustrative plates shows that IG/I2D was 1.45 (being better than import U.S. graphene product).
Embodiment 3
The discarded object coconut husk obtained from the market of farm produce is cleaned, and 95 DEG C of drying overnight, then, crushed 50 mesh sieves, be given up
Gurry coconut shell powder；In N2Under atmospheric condition, discarded object coconut shell powder is placed in tube furnace.Control programming rate for 1.0 DEG C/
Minute, 900 DEG C are warming up to, is incubated 2 hours；Continue to heat up, it is 5.0 DEG C/min to control programming rate, is warming up to 1000 DEG C, is protected
Temperature 1 hour, room temperature is slowly cooled to, cooling rate control is 5 DEG C/min, obtains the pre- carbonized product of discarded object coconut husk；
Weigh the pre- carbonized product of 2 grams of discarded object coconut husks and 6 grams of potassium hydroxide and the mixing of 2 grams of zinc chloride, then add go from
Sub- water 3mL dissolvings.Stirring dries 100 DEG C, removes water, residue is in N2Under atmospheric condition, it is placed in tube furnace.Control rises
Warm speed is 1.0 DEG C/min, is warming up to 900 DEG C, is incubated 1 hour；Continue to heat up, it is 3.0 DEG C/min to control programming rate, is risen
Temperature is incubated 0.5 hour to 1100 DEG C, slowly cools to room temperature, and cooling rate control is 5 DEG C/min, and room temperature takes out sample, uses
Deionized water is neutrality as eluant, eluent, cleaning fluid, is washed 3 times with absolute ethyl alcohol, in 60 DEG C of drying.Specific surface area is：
2186m2/ g, Raman collection of illustrative plates are determined with micro-Raman spectroscopy, [model：LabRAM Aramis manufacturers：French H.J.Y is public
Department].Raman collection of illustrative plates shows that IG/I2D was 1.95 (being better than import U.S. graphene product).
Embodiment 4
The discarded object coconut husk obtained from the market of farm produce is cleaned, and 120 DEG C of drying overnight, then, crushed 100 mesh sieves, obtain
Discarded object coconut shell powder；In N2Under atmospheric condition, discarded object coconut husk is placed in tube furnace.It is 1.0 DEG C/minute to control programming rate
Clock, 500 DEG C are warming up to, are incubated 2 hours；Continue to heat up, it is 5.0 DEG C/min to control programming rate, is warming up to 1100 DEG C, insulation 1
Hour, room temperature is slowly cooled to, cooling rate control is 5 DEG C/min, obtains the pre- carbonized product of discarded object coconut husk；
Weigh 2 grams of pre- carbonization discarded object coconut husk biomass carbons and 2 grams of Al (NO3)3Mixed with 2 grams of zinc chloride, then add and go
Ionized water 5mL dissolves.Stirring dries 100 DEG C, removes water, residue is in N2Under atmospheric condition, it is placed in tube furnace.Control
Programming rate is 1.0 DEG C/min to 500 DEG C, is incubated 2 hours；Continue to heat up, it is 5.0 DEG C/min that heating, which controls speed, heating
To 1100 DEG C, 1 hour is incubated, slowly cools to room temperature, cooling rate control is 5 DEG C/min, and room temperature takes out sample, uses diluted acid
With deionized water as eluant, eluent, until cleaning fluid is neutrality, wash 3 times with absolute ethyl alcohol, dried at 60 DEG C.After testing, institute
Obtaining product specific surface area is：2245m2/ g, Raman collection of illustrative plates are determined with micro-Raman spectroscopy, [model：LabRAM Aramis give birth to
Produce producer：French H.J.Y companies].Raman collection of illustrative plates shows that IG/I2D is 2.01 (suitable with import U.S. graphene product).
Embodiment 5：
The discarded object coconut husk obtained from the market of farm produce is cleaned, and 115 DEG C of drying overnight, then, crushed 50 mesh sieves, be given up
Gurry coconut shell powder；In N2Under atmospheric condition, discarded object coconut shell powder is placed in tube furnace.Control programming rate for 0.5 DEG C/
Minute, 800 DEG C are warming up to, is incubated 2 hours；Continue to heat up, it is 5.0 DEG C/min to control programming rate, is warming up to 950 DEG C, insulation
1 hour, room temperature is slowly cooled to, cooling rate control is 5 DEG C/min, obtains the pre- carbonized product of discarded object coconut husk；
Weigh the pre- carbonized product of 2 grams of discarded object coconut husks and 2 grams of Zn (NO3)2Mixed with 2 grams of zinc chloride, then add deionization
Water 4mL dissolves.Stirring dries 120 DEG C, removes water, residue is in N2Under atmospheric condition, it is placed in tube furnace.Control heating
Speed is 1.0 DEG C/min, is warming up to 850 DEG C, is incubated 2 hours；Continue to heat up, it is 3.0 DEG C/min to control programming rate, heating
To 1200 DEG C, be incubated 1 hour, slowly cool to room temperature, cooling rate control is 5 DEG C/min, and room temperature takes out sample, spend from
Sub- water is neutrality as eluant, eluent, cleaning fluid, is washed 3 times with absolute ethyl alcohol, in 60 DEG C of drying.Specific surface area is：2186m2/ g,
Raman collection of illustrative plates is determined with micro-Raman spectroscopy, [model：LabRAM Aramis manufacturers：French H.J.Y companies].Raman
Collection of illustrative plates shows that IG/I2D is 2.25 (suitable with import U.S. graphene product).
Present invention finds the preparation method of discarded object coconut husk biomass graphene, realizes and becomes discarded object as useful electricity
Sub- material.
From discarded object coconut husk biomass graphene prepared by embodiment, the present invention, IG/I2D is 1.25~2.31, and
And 2D peaks are into unimodal；It is multi-layer graphene that the present invention prepares biomass graphene with discarded object coconut husk, is relative to graphite powder
The oxidation-reduction method that graphene prepared by raw material uses, substantial amounts of acid waste water cause huge pollution to environment, if using
Caused waste water will necessarily consume huge manpower and financial resources cost in traditional method of wastewater treatment processing production process so that
Graphene holds at high price, and seriously hinders large-scale application and the popularization of graphene.The inventive method has significant ring
Guarantor's advantage, cost advantage and technique simplify advantage.
The graphene that the present invention obtains can be used for conductive carbon paste, ultracapacitor, the electrode material of lithium ion battery, also may be used
To be added in resin, rubber, the physical property of reinforced resin, rubber etc..Simple production process of the present invention, cost is cheap, peace
Loopful is protected, it is possible to achieve continuous industrial production, has wide market application foreground.
Claims (10)
- A kind of 1. method for preparing nitrogenous grapheme material using chitosan for raw material, it is characterised in that including following step 1, one kind The method that grapheme material is prepared using discarded object coconut husk as raw material, it is characterised in that comprise the following steps：1) dried discarded object coconut husk is crushed, obtains discarded object coconut shell powder；2) by discarded object coconut shell powder obtained by step 1), in N2Under atmospheric condition, it is warming up to 450-800 DEG C and is incubated 1~2 hour；After It is continuous to be warming up to 800~1000 DEG C, 0.5~2 hour is incubated, is slowly dropped to 25~35 DEG C, obtains the pre- carbonized product of coconut husk；3) pre- carbonized product obtained by step 2) is mixed with reaction raw materials, the weight ratio of pre- carbonized product and reaction raw materials is 1：1 ~5, in N2Under atmospheric condition, it is warming up to 800~900 DEG C and is incubated 1~2 hour；Continue to be warming up to 900~1200 DEG C, insulation 0.5 ~2 hours, room temperature is slowly dropped to, obtains discarded object coconut husk biomass graphene；The reaction raw materials be Lvization Xin ﹑ zinc nitrates and One or more in potassium hydroxide.
- 2. the method according to claim 1 that grapheme material is prepared using discarded object coconut husk as raw material, it is characterised in that institute State be warming up to 450-800 DEG C control programming rate be 0.5~2.0 DEG C/min.
- 3. the method according to claim 1 that grapheme material is prepared using discarded object coconut husk as raw material, it is characterised in that institute State and continue to be warming up to 900~1200 DEG C, it is 3.0~5.0 DEG C/min to control programming rate.
- 4. the method according to claim 1 that grapheme material is prepared using discarded object coconut husk as raw material, it is characterised in that step It is rapid 2) described to be slowly dropped to 25~35 DEG C and the step 3) room temperature that is slowly dropped to control cooling rate as 3~5 DEG C/min.
- 5. the method according to claim 1 that grapheme material is prepared using discarded object coconut husk as raw material, it is characterised in that institute It is that will be left discarded coconut husk after edible coconut by obtained by 95~120 DEG C of baking 12-24 hours to state dry discarded object coconut husk.
- 6. the method according to claim 1 that grapheme material is prepared using discarded object coconut husk as raw material, it is characterised in that step Rapid 3) described cool to after room temperature also includes taking out sample, by the use of deionized water as eluant, eluent, cleans as neutrality, uses absolute ethyl alcohol Washing is multiple, 100-120 DEG C of drying.
- 7. the method according to claim 1 that grapheme material is prepared using discarded object coconut husk as raw material, it is characterised in that step The specific surface area of rapid 3) gained discarded object coconut husk biomass graphene is 1170~2673m2/g。
- 8. the method according to claim 1 that grapheme material is prepared using discarded object coconut husk as raw material, it is characterised in that step The D ﹑ G and 2D peaks of the Raman spectrum of rapid 3) gained discarded object coconut husk biomass graphene are unimodal；And IG/I2D be 1.25~ 2.31。
- 9. the method according to claim 1 that grapheme material is prepared using discarded object coconut husk as raw material, it is characterised in that step It is rapid 1) to obtain also including sieving after discarded object coconut shell powder；The sieving was 50~100 mesh sieves.
- 10. the method according to claim 1 that grapheme material is prepared using discarded object coconut husk as raw material, it is characterised in that Step 2), which is warming up to 450-800 DEG C and is incubated 1~2 hour, to be carried out in tube furnace；Step 3) is warming up to 800~900 DEG C of insulations 1 ~2 hours are carried out in tube furnace.
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| CN110387099A (en) * | 2019-07-18 | 2019-10-29 | 华南理工大学 | A kind of tealeaf residue graphene-CuCeMOF-PVB composite material and preparation method and application |
| CN110408155A (en) * | 2019-07-18 | 2019-11-05 | 华南理工大学 | A kind of agricultural mulching graphene-CuCo-PVB composite material and preparation method and application |
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| CN111686761A (en) * | 2020-05-20 | 2020-09-22 | 华南理工大学 | Cu/CdS/graphene composite photocatalyst and preparation method and application thereof |
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