CN108249426A - A kind of method that biomass graphene is prepared using Chinese medicine slag as utilization of carbon source hydro-thermal method - Google Patents
A kind of method that biomass graphene is prepared using Chinese medicine slag as utilization of carbon source hydro-thermal method Download PDFInfo
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Abstract
The invention discloses a kind of method that biomass graphene is prepared using Chinese medicine slag as utilization of carbon source hydro-thermal method, step is：(1) Chinese medicine discards the dregs of a decoction and biomass fuel is made, and burning obtains biomass carbon；(2) by biomass carbon heating and calcining, biomass graphite is obtained；(3) graphene is made by hydro-thermal method in biomass graphite.The present invention is using waste residue of Chinese herbs as raw material, and existing biomass fuel process compatible, and then is graphitized, then the preparation process of the method synthesising biological matter graphene using hydro-thermal with the carbon that biomass fuel combustion obtains, and can greatly reduce energy consumption.Present invention process is simple, at low cost, yield is high, production security is strong, required instrument and equipment is simple, without catalyst, environmentally safe, easily realize industrialized production, simultaneously, the dregs of a decoction are discarded as carbon source using Chinese medicine, it derives from a wealth of sources, it can realize that Chinese medicine discards the comprehensive utilization of the dregs of a decoction, reduce production cost, there is preferable compatibility with the existing production technology in pharmaceutical factory.
Description
Technical field
The invention belongs to technical field of graphene preparation, specially one kind is prepared using Chinese medicine slag as carbon source using hydro-thermal method
The method of biomass graphene.
Background technology
It is the solid waste generated in herbal pharmaceutical production process that Chinese medicine, which discards the dregs of a decoction, mostly the root of plant, stem, leaf
It is formed, contains a large amount of cellulose, hemicellulose, lignin etc..At present, Chinese medicine cultivated area in China's is public for more than 240 ten thousand
Hectare, about 70,000,000 tons of medicinal material annual output.During process deeply industry is carried out, the solid waste such as generated dregs of a decoction are unexpectedly
There are 35,000,000 tons.If things go on like this, the serious waste of natural resources of Chinese medicinal materials had both been caused, has also brought huge pressure to ecological environment
Power.In addition to the Chinese medicine waste in production process, the dregs of a decoction can be also generated when boiling medicine, these dregs of a decoction are dealt with improperly, will also result in
Environmental pollution.
Graphene (Graphene) be one kind by carbon atom with sp2Hybridized orbit composition hexangle type is in the two dimension of honeycomb lattice
Carbon nanomaterial, with excellent optics, electricity, mechanical characteristic, in materialogy, micro-nano technology, the energy, biomedicine and medicine
Object transmission etc. has important application prospect, it is considered to be a kind of future revolutionary material.At present, synthesizing graphite alkene
Using there are mainly two types of more in method：One kind is chemical vapour deposition technique (CVD), and another kind is reduction-oxidation graphite method.
The graphene of CVD method production is suitable for doing electronic device, but usually requires harsh reaction condition, expensive equipment, longer
Period, relatively low yield, be not suitable for be similar to electrode material field large-scale application.Required for reduction-oxidation graphite method
The dosage of strong oxidizer (concentrated sulfuric acid, potassium permanganate etc.) is tens times of graphite raw material, causes environmental pollution serious.Production cost
It is high, so as to greatly limit the process of its industrialization.
In conclusion existing graphene preparation method is there are complex process, production security is poor, production cost is high, reaction
The problems such as required equipment complexity, severe reaction conditions, low output, so as to be difficult to industrialized production.
Invention content
In order to overcome the shortcomings and deficiencies of the prior art described above, the purpose of the present invention is to provide one kind using Chinese medicine slag as carbon
The method that source prepares biomass graphene using hydro-thermal method, it is simple for process, it is environmentally safe, and realize that Chinese medicine discards the dregs of a decoction
Comprehensive utilization.
The purpose of the present invention is realized by following proposal：One kind prepares biomass stone by utilization of carbon source hydro-thermal method of Chinese medicine slag
The method of black alkene, includes the following steps：
(1) Chinese medicine discards the dregs of a decoction and is ground into powder, and drying is simultaneously squeezed into biomass fuel, and burning occurs carbonization and obtains biology
Matter carbon；
(2) biomass carbon heating and calcining is realized and be graphitized, obtain biomass graphite；
(3) biomass graphite is added in the NaCl solution of a concentration of 0.0075-0.0175g/ml and impregnates 2-6h, and in
Have in the reaction kettle of stainless steel inner container and carry out hydro-thermal reaction 10-14h at 200-400 DEG C, be cooled to room temperature after reaction, remove
Liner obtains graphene mixed liquor, after filtering, deionized water washing, absolute ethyl alcohol washing repeatedly, is drying to obtain graphene.
Chinese medicine in the step (1) discards the dregs of a decoction and is selected from radix bupleuri, Radix Isatidis, kuh-seng, Radix Salviae Miltiorrhizae, Radix Glycyrrhizae, Radix Astragali, chicken blood
Rattan, sargentodoxa cuneata, Ramulus Taxilli, the root bark of white mulberry, moutan bark, Cortex Eucommiae, cortex albiziae, erythrina bark, the root bark of shaggy-fruited dittany, white backleaf mallotus root, redback christmashush root, the leaves of pulse plants
The one or more of perfume (or spice) etc..
In the step (1), burning carbonate temperature is 600 DEG C or more.
Heating and calcining temperature in the step (2) is 1000 DEG C or more.
In the step (3), 3g graphite is added in by 0.6-1.4g NaCl constant volumes in the solution of 80mL deionized waters
2-6h is impregnated, is placed in the reaction kettle of the 100mL specifications equipped with stainless steel inner container, in 200-400 DEG C of hydro-thermal reaction 10-14h,
It is cooled to room temperature after reaction, removal liner obtains graphene mixed liquor, by filtering, deionized water washing, absolute ethyl alcohol
After washing repeatedly, it is drying to obtain graphene.
Preferably, the graphite levels described in step (3) are 3g, and NaCl dosages are 1.0g, with 80mL deionized water constant volumes,
It is 4h to be placed in soaking time in the reaction kettle of the stainless steel inner container of 100mL specifications, and hydrothermal temperature is 300 DEG C, the reaction time
For 12h.
The present invention is using waste residue of Chinese herbs as raw material, and existing biomass fuel process compatible, and then is fired with biomass fuel
The carbon obtained is burnt to be graphitized, then the preparation process of the method synthesising biological matter graphene using hydro-thermal, it can be by a relatively large margin
Ground reduces energy consumption.Present invention process is simple, at low cost, yield is high, production security is strong, required instrument and equipment is simple, nothing is urged
It is agent, environmentally safe, easily realize industrialized production, meanwhile, the dregs of a decoction are discarded as carbon source using Chinese medicine, are derived from a wealth of sources, Neng Goushi
Existing Chinese medicine discards the comprehensive utilization of the dregs of a decoction, reduces production cost, has preferable compatibility with the existing production technology in pharmaceutical factory.
Description of the drawings
Fig. 1 is transmission electron microscope (TEM) photo of the biomass graphene obtained by the embodiment of the present invention 1；
Fig. 2 is Raman spectrum (wherein, the 1580cm of the biomass graphene obtained by the embodiment of the present invention 1-1With
2700cm-1Characteristic peak for graphene).
Specific embodiment
The present invention is a kind of method that biomass graphene is prepared using Chinese medicine slag as utilization of carbon source hydro-thermal method, including following
Step：
(1) Chinese medicine discards the dregs of a decoction and is ground into powder, and drying is simultaneously squeezed into biomass fuel, and burning occurs carbonization and obtains biology
Matter carbon.Preferably, Chinese medicine discards the dregs of a decoction and is selected from radix bupleuri, Radix Isatidis, kuh-seng, Radix Salviae Miltiorrhizae, Radix Glycyrrhizae, Radix Astragali, Caulis Spatholobi, sargentodoxa cuneata, mulberry
One kind of parasitism, the root bark of white mulberry, moutan bark, Cortex Eucommiae, cortex albiziae, erythrina bark, the root bark of shaggy-fruited dittany, white backleaf mallotus root, redback christmashush root, wrinkled giant hyssop etc. or
More than one.Preferably, burning carbonate temperature is 600 DEG C or more.
(2) biomass carbon heating and calcining is realized and be graphitized, obtain biomass graphite.Preferably, heating and calcining temperature is
1000 DEG C or more.
(3) biomass graphite is added in the NaCl solution of a concentration of 0.0075-0.0175g/ml and impregnates 2-6h, and in
Have in the reaction kettle of stainless steel inner container and carry out hydro-thermal reaction 10-14h at 200-400 DEG C, be cooled to room temperature after reaction, remove
Liner obtains graphene mixed liquor, after filtering, deionized water washing, absolute ethyl alcohol washing repeatedly, is drying to obtain graphene.
Preferably, the addition of 3g graphite is impregnated into 2-6h in the solution of 80mL deionized waters by 0.6-1.4g NaCl constant volumes, is placed in matching
Have in the reaction kettle of 100mL specifications of stainless steel inner container, in 200-400 DEG C of hydro-thermal reaction 10-14h, be cooled to after reaction
Room temperature, removal liner obtain graphene mixed liquor, and after filtering, deionized water washing, absolute ethyl alcohol washing repeatedly, drying is
Obtain graphene.It is furthermore preferred that graphite levels are 3g, NaCl dosages are 1.0g, with 80mL deionized water constant volumes, are placed in 100mL rule
Soaking time is 4h in the reaction kettle of the stainless steel inner container of lattice, and hydrothermal temperature is 300 DEG C, reaction time 12h.
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
Embodiment 1
The present embodiment is completed by following step：
(1) radix bupleuri is discarded into the dregs of a decoction and is broken into powder, drying is simultaneously squeezed into cylindrical biomass fuel, can be applied to biology
Matter fuel boiler is to meet needs of the pharmaceutical factory production technology to heating power.In 600 DEG C of burning carbonizations, biomass carbon is obtained；
(2) biomass carbon is placed in high temperature furnace in 1000 DEG C of heating and calcinings, realizes graphitization；
(3) 3g graphite and 1.0g NaCl are added in the 100mL specification reaction kettles for filling 80mL deionized waters, impregnated
4h in 300 DEG C of hydro-thermal reaction 12h, is cooled to room temperature after reaction, then filters, obtained solid is washed, is drying to obtain stone
Black alkene, TEM photos are as shown in Figure 1, Raman spectrum is as shown in Figure 2.
Embodiment 2
The present embodiment is completed by following step：
(1) redback christmashush root is discarded into the dregs of a decoction and is broken into powder, drying is simultaneously squeezed into cylindrical biomass fuel, in 800 DEG C of combustions
Carbonization is burnt, obtains biomass carbon；
(2) biomass carbon is realized into graphitization in 1200 DEG C of heating and calcinings；
(3) 3g graphite and 1.4g NaCl are added in the 100mL specification reaction kettles for filling 80mL deionized waters, impregnated
4h in 250 DEG C of hydro-thermal reaction 13h, is cooled to room temperature after reaction, then filters, obtained solid is washed, is drying to obtain stone
Black alkene.
Embodiment 3
The present embodiment is completed by following step：
(1) Radix Glycyrrhizae, wrinkled giant hyssop are discarded into the dregs of a decoction and is broken into powder, drying is simultaneously squeezed into cylindrical biomass fuel, in 600 DEG C of combustions
Carbonization is burnt, obtains biomass carbon；
(2) biomass carbon is realized into graphitization in 1000 DEG C of heating and calcinings；
(3) 3g graphite and 0.8g NaCl are added in the 100mL specification reaction kettles for filling 80mL deionized waters, impregnated
2h in 300 DEG C of hydro-thermal reaction 12h, is cooled to room temperature after reaction, then filters, obtained solid is washed, is drying to obtain stone
Black alkene.
Embodiment 4
The present embodiment is completed by following step：
(1) Radix Isatidis is discarded into the dregs of a decoction and is broken into powder, drying is simultaneously squeezed into cylindrical biomass fuel, can be applied to give birth to
Biomass fuel boiler is to meet needs of the pharmaceutical factory production technology to heating power.In 600 DEG C of burning carbonizations, biomass carbon is obtained；
(2) biomass carbon is placed in high temperature furnace in 1000 DEG C of heating and calcinings, realizes graphitization；
(3) 3g graphite and 1.2g NaCl are added in the 100mL specification reaction kettles for filling 80mL deionized waters, impregnated
6h in 300 DEG C of hydro-thermal reaction 12h, is cooled to room temperature after reaction, then filters, obtained solid is washed, is drying to obtain stone
Black alkene, TEM photos are as shown in Figure 1, Raman spectrum is as shown in Figure 2.
Claims (6)
1. a kind of method that biomass graphene is prepared using Chinese medicine slag as utilization of carbon source hydro-thermal method, includes the following steps：
(1) Chinese medicine discards the dregs of a decoction and is ground into powder, and drying is simultaneously squeezed into biomass fuel, and burning occurs carbonization and obtains biomass
Carbon；
(2) biomass carbon heating and calcining is realized and be graphitized, obtain biomass graphite；
(3) biomass graphite is added in the NaCl solution of a concentration of 0.0075-0.0175g/ml and impregnates 2-6h, and in equipped with not
Hydro-thermal reaction 10-14h is carried out at 200-400 DEG C in the reaction kettle of rust steel liner, is cooled to room temperature after reaction, removes liner
Graphene mixed liquor is obtained, after filtering, deionized water washing, absolute ethyl alcohol washing repeatedly, is drying to obtain graphene.
2. the method according to claim 1 that biomass graphene is prepared using Chinese medicine slag as utilization of carbon source hydro-thermal method, special
Sign is：Chinese medicine in the step (1) discard the dregs of a decoction be selected from radix bupleuri, Radix Isatidis, kuh-seng, Radix Salviae Miltiorrhizae, Radix Glycyrrhizae, Radix Astragali, Caulis Spatholobi,
Sargentodoxa cuneata, Ramulus Taxilli, the root bark of white mulberry, moutan bark, Cortex Eucommiae, cortex albiziae, erythrina bark, the root bark of shaggy-fruited dittany, white backleaf mallotus root, redback christmashush root, wrinkled giant hyssop
One or more.
3. the method according to claim 1 that biomass graphene is prepared using Chinese medicine slag as utilization of carbon source hydro-thermal method, special
Sign is：In the step (1), burning carbonate temperature is 600 DEG C or more.
4. the method according to claim 1 that biomass graphene is prepared using Chinese medicine slag as utilization of carbon source hydro-thermal method, special
Sign is：Heating and calcining temperature in the step (2) is 1000 DEG C or more.
5. the method according to claim 1 that biomass graphene is prepared using Chinese medicine slag as utilization of carbon source hydro-thermal method, special
Sign is：In the step (3), 3g graphite is added in by 0.6-1.4g NaCl constant volumes in the solution of 80mL deionized waters
2-6h is impregnated, is placed in the reaction kettle of the 100mL specifications equipped with stainless steel inner container, in 200-400 DEG C of hydro-thermal reaction 10-14h,
It is cooled to room temperature after reaction, removal liner obtains graphene mixed liquor, by filtering, deionized water washing, absolute ethyl alcohol
After washing repeatedly, it is drying to obtain graphene.
6. the method according to claim 5 that biomass graphene is prepared using Chinese medicine slag as utilization of carbon source hydro-thermal method, special
Sign is：In the step (3), graphite levels 3g, NaCl dosage are 1.0g, with 80mL deionized water constant volumes, are placed in
Soaking time is 4h in the reaction kettle of the stainless steel inner container of 100mL specifications, and hydrothermal temperature is 300 DEG C, and the reaction time is
12h。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111330596A (en) * | 2020-03-09 | 2020-06-26 | 内蒙古工业大学 | Solid acid catalyst and preparation method and application thereof |
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Application publication date: 20180706 |