CN108059146A - A kind of method that low-temperature hydrothermal prepares Carbon Materials - Google Patents

A kind of method that low-temperature hydrothermal prepares Carbon Materials Download PDF

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Publication number
CN108059146A
CN108059146A CN201810040509.7A CN201810040509A CN108059146A CN 108059146 A CN108059146 A CN 108059146A CN 201810040509 A CN201810040509 A CN 201810040509A CN 108059146 A CN108059146 A CN 108059146A
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China
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carbon materials
temperature
low
hydro
quality
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CN201810040509.7A
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Chinese (zh)
Inventor
唐志红
张芝文
杨俊和
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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Priority to CN201810040509.7A priority Critical patent/CN108059146A/en
Publication of CN108059146A publication Critical patent/CN108059146A/en
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Abstract

The present invention provides a kind of methods that low-temperature hydrothermal prepares Carbon Materials, water-soluble carbon source is configured to aqueous solution, the carbon source is any one in glucose, sucrose, fructose, maltose, lactose, starch, xylose or lignocellulosic, the concentration of the aqueous solution is 1 1000g/l, is then uniformly mixed with graphene oxide and obtains mixed liquor;The quality of the graphene oxide is 0.001% the 10% of carbon source quality;Mixed liquor is placed in water heating kettle, at a temperature of 80 160 DEG C, hydro-thermal reaction 1 is for 24 hours;Carbon Materials will be obtained after the sample washing of preparation, drying, in obtained Carbon Materials, the mass percentage of the charcoal is 50% to 80%.The present invention is realized under low temperature(Minimum 80 DEG C)Hydro-thermal charing prepares Carbon Materials, and the method for the present invention is simple, and energy saving, can reduce cost.

Description

A kind of method that low-temperature hydrothermal prepares Carbon Materials
Technical field
The invention belongs to chemical fields, are related to a kind of Carbon Materials, and specifically a kind of low-temperature hydrothermal prepares Carbon Materials Method.
Background technology
Hydro-thermal charing is a kind of common method for preparing Carbon Materials, since hydro-thermal charing is carried out under aqueous solution, anti- Answer in dehydration, will release itself 1/3rd Combustion Energy, therefore there is high-energy and high-efficiency.In addition hydro-thermal carbonizes Equipment is simple, and easy to operate and biomass carbon yield is higher, is a kind of green, sustainable production charcoal approach.Usual hydro-thermal charcoal Change temperature and be generally greater than 180 DEG C, this proposes the Preparation equipment of material certain requirement, also, hydro-thermal reaction is in sealing Under the conditions of carry out, too there is also security risks for high-temperature.
The content of the invention
For above-mentioned technical problem of the prior art, the present invention provides the sides that a kind of low-temperature hydrothermal prepares Carbon Materials Method, this low-temperature hydrothermal prepare Carbon Materials method to solve to prepare in the prior art Carbon Materials method temperature it is too high There is technical issues that.
The present invention provides a kind of methods that low-temperature hydrothermal prepares Carbon Materials, include the following steps:
1) water-soluble carbon source is configured to aqueous solution, the carbon source is glucose, sucrose, fructose, maltose, lactose, shallow lake Any one in powder, xylose or lignocellulosic, the concentration of the aqueous solution is 1-1000g/l, then with aoxidizing stone Black alkene, which is uniformly mixed, obtains mixed liquor;The quality of the graphene oxide is the 0.001%-10% of carbon source quality;
2) mixed liquor is placed in water heating kettle, at a temperature of 80-160 DEG C, hydro-thermal reaction 1-24h;
3) by step 2)The sample of preparation washs, obtains Carbon Materials after drying, in obtained Carbon Materials, the quality of the charcoal Percentage composition is 50% to 80%.
Further, step 2)Temperature be 80 ~ 100 DEG C.
Further, the concentration of the aqueous solution is 400-500g/l.
Further, step 2)Temperature be between 100 DEG C to 160 DEG C;When reaction time is 10-16 small.
Further, carbon source is preferably dextrose and saccharose.
Further, glucose is configured to the solution of 100g/l, addition and the oxygen that glucose quality percentage is 0.1% Graphite alkene is uniformly mixed and obtains mixed liquor;Mixed liquor is placed in 100 DEG C of reaction 12h in water heating kettle, by product deionization Water is dried after fully washing and can obtain hydro-thermal Carbon Materials, and the mass percentage of charcoal is 62% in hydro-thermal Carbon Materials.
The present invention is not only realized at lower temperatures by adding in graphene oxide(Minimum 80 DEG C)Hydro-thermal charing system Standby Carbon Materials, and graphene oxide or graphene also change as a kind of economic, efficient catalyst after hydro-thermal carbonizes For Carbon Materials, so as to solve the problems, such as catalyst recycling and purification of products.Graphene oxide or graphene are serving as catalysis Also template is provided to be biomass carbonated so that the Carbon Materials of preparation have very high specific surface area, have expanded it while agent Application field.
The present invention is compared with prior art, and technological progress is significant.The more conventional hydro-thermal charing method of the present invention, can Effectively reduce hydro-thermal carbonization temperature.The present invention can not only convert biomass into Carbon Materials under cryogenic, but also save Utilize the purified treatment step of other catalyst., can not only be energy saving present invention reduces hydro-thermal carbonization temperature, and Safer, the requirement to equipment is relatively low.
Description of the drawings
Fig. 1 is the Carbon Materials sample drawing according to prepared by the method for the present invention at 100 DEG C.
Fig. 2 is the Carbon Materials sample drawing according to prepared by the method for the present invention at 120 DEG C.
Fig. 3 is the Carbon Materials sample drawing according to prepared by the method for the present invention at 140 DEG C.
Fig. 4 is the Carbon Materials sample drawing according to prepared by the method for the present invention at 160 DEG C.
Specific embodiment
The present invention is further illustrated below by embodiment.These embodiments are merely to illustrate the present invention and do not have to In limiting the scope of the invention.In addition, after present disclosure has been read, those skilled in the art can make the present invention Similar change or modification, these equivalent forms also fall within the scope of the appended claims of the present application.
Embodiment 1
The glucose solution 35ml of 20g/l is taken, addition mass percent is 0.1% graphene oxide, is uniformly mixed and is placed on volume For in the water heating kettle of 50ml, it to be reacted to 16h at 100 DEG C, collecting reaction product obtains Carbon Materials sample, is detected by XPS The carbon content of resulting materials is 52%, as shown in Figure 1.It is anti-at identical temperature in the presence of the left side is no graphene oxide Carbon Materials are not obtained after answering;After 0.1% graphene oxide of the right for addition glucose quality, the product char of black can be obtained.
Embodiment 2
Take the sucrose solution 35ml of 200g/l, addition mass percent is 1% graphene oxide, is uniformly mixed and is placed on volume and is In the water heating kettle of 50ml, it is reacted to 8h at 120 DEG C, collecting reaction product obtains Carbon Materials sample, as obtained by XPS detections The carbon content of material is 60%.As shown in Figure 2.The left side be no graphene oxide in the presence of, at identical temperature react after Carbon Materials are not obtained;After 1% graphene oxide of the right for addition sucrose quality, the product char of black can be obtained.
Embodiment 3
Take the fructose soln 35ml of 500g/l, addition mass percent is 5% graphene oxide, is uniformly mixed and is placed on volume and is In the water heating kettle of 50ml, it is reacted to 20h at 140 DEG C, collecting reaction product obtains Carbon Materials sample, and institute is detected by XPS The carbon content for obtaining material is 72%.As shown in Figure 3.The left side is the production that is obtained after reaction in the presence of no graphene oxide Object.The product that the right obtains after the graphite oxide alkene reaction for addition fructose quality 5%.
Embodiment 4
Take the lactose solution 35ml of 800g/l, addition mass percent is 7% graphene oxide, is uniformly mixed and is placed on volume and is In the water heating kettle of 50ml, it is reacted to 5h at 160 DEG C, collecting reaction product obtains Carbon Materials sample, as obtained by XPS detections The carbon content of material is 68%.As shown in Figure 4.The left side is the production that is obtained after reaction in the presence of no graphene oxide Object.The product that the right obtains after the graphite oxide alkene reaction for addition lactose quality 8%.

Claims (6)

1. a kind of method that low-temperature hydrothermal prepares Carbon Materials, it is characterised in that include the following steps:
1)Water-soluble carbon source is configured to aqueous solution, the carbon source is glucose, sucrose, fructose, maltose, lactose, shallow lake Any one in powder, xylose or lignocellulosic, the concentration of the aqueous solution is 1-1000g/l, then with aoxidizing stone Black alkene, which is uniformly mixed, obtains mixed liquor;The quality of the graphene oxide is the 0.001%-10% of carbon source quality;
2)Mixed liquor is placed in water heating kettle, at a temperature of 80-160 DEG C, hydro-thermal reaction 1-24h;
3)By step 2)The sample of preparation washs, obtains Carbon Materials after drying, in obtained Carbon Materials, the quality of the charcoal Percentage composition is 50% to 80%.
2. the method that a kind of low-temperature hydrothermal according to claim 1 prepares Carbon Materials, it is characterised in that:Step 2)Temperature For 80 ~ 100 DEG C.
3. the method that a kind of low-temperature hydrothermal according to claim 1 prepares Carbon Materials, it is characterised in that:The aqueous solution Concentration be 400-500g/l.
4. the method that a kind of low-temperature hydrothermal according to claim 1 prepares Carbon Materials, it is characterised in that:Step 2)Temperature For between 100 DEG C to 160 DEG C;When reaction time is 10-16 small.
5. the method that a kind of low-temperature hydrothermal according to claim 1 prepares Carbon Materials, it is characterised in that:Carbon source is glucose Or sucrose.
6. the method that a kind of low-temperature hydrothermal according to claim 1 prepares Carbon Materials, it is characterised in that:Glucose is prepared Into the solution of 100g/l, it is 0.1% graphene oxide to add in glucose quality percentage, is uniformly mixed and obtains mixed liquor; Mixed liquor is placed in 100 DEG C of reaction 12h in water heating kettle, it is dry after product is fully washed with deionized water to can obtain hydro-thermal charcoal Material, the mass percentage of charcoal is 62% in hydro-thermal Carbon Materials.
CN201810040509.7A 2018-01-16 2018-01-16 A kind of method that low-temperature hydrothermal prepares Carbon Materials Pending CN108059146A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110092640A (en) * 2019-05-30 2019-08-06 福建省威尔陶瓷股份有限公司 A kind of high heat resistanceheat resistant, shock resistance domestic ceramics and preparation method thereof
CN113086966A (en) * 2021-04-09 2021-07-09 安徽工业大学 Method for preparing carbon material by converting sucrose waste liquid

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102718210A (en) * 2012-07-03 2012-10-10 新疆大学 Method for preparing graphene oxide three-dimensional self-assembled aerogel and application of graphene oxide three-dimensional self-assembled aerogel
CN104772118A (en) * 2015-04-24 2015-07-15 河北工业大学 Hydrophilic graphene based carbon material and application thereof
CN103201216B (en) * 2010-12-31 2015-07-22 海洋王照明科技股份有限公司 Composite material of carbon-coated graphene oxide, preparation method and application thereof

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Publication number Priority date Publication date Assignee Title
CN103201216B (en) * 2010-12-31 2015-07-22 海洋王照明科技股份有限公司 Composite material of carbon-coated graphene oxide, preparation method and application thereof
CN102718210A (en) * 2012-07-03 2012-10-10 新疆大学 Method for preparing graphene oxide three-dimensional self-assembled aerogel and application of graphene oxide three-dimensional self-assembled aerogel
CN104772118A (en) * 2015-04-24 2015-07-15 河北工业大学 Hydrophilic graphene based carbon material and application thereof

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110092640A (en) * 2019-05-30 2019-08-06 福建省威尔陶瓷股份有限公司 A kind of high heat resistanceheat resistant, shock resistance domestic ceramics and preparation method thereof
CN113086966A (en) * 2021-04-09 2021-07-09 安徽工业大学 Method for preparing carbon material by converting sucrose waste liquid

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