CN107804834A - A kind of preparation method of molasses base hydro-thermal charcoal - Google Patents
A kind of preparation method of molasses base hydro-thermal charcoal Download PDFInfo
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- CN107804834A CN107804834A CN201711114685.2A CN201711114685A CN107804834A CN 107804834 A CN107804834 A CN 107804834A CN 201711114685 A CN201711114685 A CN 201711114685A CN 107804834 A CN107804834 A CN 107804834A
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Abstract
The present invention relates to a kind of preparation method of molasses base hydro-thermal charcoal, belong to biomass absorbent field of material technology.The present invention is used as template using nanosized silica particles, L-cysteine is as hetero atom N, S source, doping N is made by hydro-thermal method, the high-specific surface area hydro-thermal Carbon Materials of S elements, and activated using potassium carbonate, this method activation condition is gentle, enter the etching in material internal generation hole by scattering and permeating, promote layer of charcoal separation, course of reaction is easy to control, and equipment corrosion and the intoxicating sex chromosome mosaicism that may trigger can be avoided, obtained molasses base hydro-thermal charcoal has flourishing pore structure, cavernous structure physically well develops, in graphitic layers pile structure, the ability that material transmits electronics can be improved, contain-NH in surface2,-SH isoreactivity groups, good surface-active and heat endurance are made it have, there is excellent electric double layer energy-storage property.
Description
Technical field
The present invention relates to a kind of preparation method of molasses base hydro-thermal charcoal, belong to biomass absorbent field of material technology.
Background technology
Hydro-thermal charing is low with reaction temperature, and raw material is not limited by moisture, and power consumption is few, CO2It is few etc. excellent to change burst size
Point, it is a kind of efficient biomass preprocessing means and biomass full constituent method for transformation.The biomass materials such as straw, timber have
There is the features such as source is wide, yield is high, effective rate of utilization is low.Therefore, it is hydro-thermal charring is renewable for handling straw timber etc.
Biomass resource, production high added value material-hydro-thermal charcoal are significant.
Biomass is converted into hydro-thermal charcoal and depends on activation process.For physically activated, chemical activation has step
The advantages that rapid simple, carbonization and activation can simultaneously be carried out, can reacted at a lower temperature, chemical activating agent recoverable, and
And chemical activation can prepare the hydro-thermal charcoal of performance relative good, but its activator used is applied in food and medicine field
In may trigger it is causing toxicity, can corrosion reaction equipment, and react violent, be difficult to control.
The raw material for preparing biomass by hydro-thermal charcoal at present is mainly glucose, pentosan, cellulose, hemicellulose and lignin
It is higher Deng biomass components or micromolecular compound, time related cost.Molasses are sugar refinery discarded object, and composition is more complicated, because
It is unfavorable for directly utilizing for stickiness height.At present, molasses are used primarily in fermentation arts, and progress fermentation process is ineffective, and its
The secondary pollution problem (processing of such as vinasse) that fermented product is brought is remained unsolved, and environmental pollution is caused if directly discarding, by
Carbon content is enriched in molasses, if finding suitable method molasses prepares Functional carbon material, can not only solve sugaring enterprise
The puzzlement of industry, can also be that the preparation of hydro-thermal carbon is sought
To new raw material, therefore it is significant to open up the new direction that molasses utilize.
The content of the invention
The technical problems to be solved by the invention：Environmental pollution is easily caused for molasses are difficult, and prepares water at present
The activator that hot charcoal uses may trigger causing toxicity, meeting corrosion reaction equipment in being applied in food and medicine field, and react acute
It is strong, it is difficult to control, the problem of the hydro-thermal charcoal electric property difference of preparation, there is provided a kind of preparation method of molasses base hydro-thermal charcoal.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A kind of preparation method of molasses base hydro-thermal charcoal, it is characterised in that specifically preparation process is：
（1）After molasses are diluted with water and L-cysteine, mass fraction are 20% ammoniacal liquor, tetraethyl orthosilicate stirring reaction, are obtained
Reaction solution；
（2）Reaction solution is fitted into heating response in hydrothermal reaction kettle, is cooled to take out after room temperature and filters to obtain filter residue；
（3）Filter residue is alternately washed to cleaning solution in being dried after neutrality with deionized water and absolute ethyl alcohol, obtains carbon materials material precursor；
（4）Carbon materials material precursor is immersed in solution of potassium carbonate, 4~6h is stirred at 70~80 DEG C, filters to obtain filter cake；
（5）It will be fitted into after filter cake washing and drying in Muffle furnace, under nitrogen atmosphere, 3~4h of activated sintering, obtain molasses base hydro-thermal
Charcoal.
Step（1）The molasses and the mass ratio of deionized water are 1：5.
Step（1）The molasses, L-cysteine, mass fraction are 20% ammoniacal liquor, the parts by weight of tetraethyl orthosilicate be 10 ~
20 parts of molasses, 1~2 part of L-cysteine, 2~4 parts of mass fractions are 20% ammoniacal liquor, 2~4 parts of tetraethyl orthosilicates.
Step（2）The heating response is again heated to 200~240 DEG C instead to be heated to 160~180 DEG C of 12~16h of reaction
Answer 20~30h.
Step（4）The mass fraction of the solution of potassium carbonate is 10%, and dosage is the 50 ~ 200 of carbon materials material precursor quality
Step（5）The activated sintering is to be heated to 500~600 DEG C of 3~4h of activated sintering.
Compared with other method, advantageous effects are the present invention：
The present invention source of the L-cysteine as hetero atom N, S, is passed through using nanosized silica particles as template
The high-specific surface area hydro-thermal Carbon Materials of doping N, S element are made in hydro-thermal method, and are activated using potassium carbonate, this method activation condition temperature
With, by scattering and permeating enter material internal occur hole etching, promote layer of charcoal separation, course of reaction is easy to control, and can avoid
Equipment corrosion and the intoxicating sex chromosome mosaicism that may trigger, obtained molasses base hydro-thermal charcoal have flourishing pore structure, cavernous structure
Physically well develop, in graphitic layers pile structure, the ability that material transmits electronics can be improved ,-NH is contained on surface2,-SH isoreactivities
Group, good surface-active and heat endurance are made it have, there is excellent electric double layer energy-storage property.
Embodiment
10~20g molasses are taken, are added in 50~100mL deionized waters, 20~30min is stirred with 300~400r/min, then
Add 1~2g L-cysteine, 2~4g mass fractions are 20% ammoniacal liquor, 2~4g tetraethyl orthosilicates, at 30~40 DEG C after
4~6h of continuous stirring, obtains reaction solution, reaction solution is fitted into hydrothermal reaction kettle, is heated to 160~180 DEG C of 12~16h of reaction, then
200~240 DEG C of 20~30h of reaction are heated to, is cooled to take out after room temperature and filters to obtain filter residue, handed over deionized water and absolute ethyl alcohol
For washing to cleaning solution in neutrality, it is placed in drying box, 3~5h is dried at 80~90 DEG C, carbon materials material precursor is obtained, takes 1
~2g carbon materials material precursors, be immersed in 100~200g mass fractions as in 10% solution of potassium carbonate, at 70~80 DEG C with 300~
400r/min stirs 4~6h, filters to obtain filter cake, is washed with deionized to cleaning solution in neutrality, is placed in drying box, 80~
3~5h is dried at 90 DEG C, is reloaded into Muffle furnace, under nitrogen atmosphere, is heated to 500~600 DEG C of activated sintering 3~4h, it is cold
But to after room temperature, molasses base hydro-thermal charcoal is obtained.
Example 1
10g molasses are taken, are added in 50mL deionized waters, 20min is stirred with 300r/min, adds 1g L-cysteine, 2g
Mass fraction is 20% ammoniacal liquor, 2g tetraethyl orthosilicates, continues to stir 4h at 30 DEG C, obtains reaction solution, and it is anti-that reaction solution is loaded into hydro-thermal
Answer in kettle, be heated to 160 DEG C of reaction 12h, be again heated to 200 DEG C of reaction 20h, be cooled to take out after room temperature and filter to obtain filter residue, use
Alternately washing to cleaning solution is in neutrality for deionized water and absolute ethyl alcohol, is placed in drying box, 3h is dried at 80 DEG C, obtains carbon materials
Material precursor, 1g carbon materials material precursors are taken, it is in 10% solution of potassium carbonate, with 300r/ at 70 DEG C to be immersed in 100g mass fractions
Min stirs 4h, filters to obtain filter cake, is washed with deionized to cleaning solution in neutrality, is placed in drying box, is dried at 80 DEG C
3h, it is reloaded into Muffle furnace, under nitrogen atmosphere, is heated to 500 DEG C of activated sintering 3h, after being cooled to room temperature, obtains molasses Ji Shui
Hot charcoal.
Example 2
15g molasses are taken, are added in 75mL deionized waters, 25min is stirred with 350r/min, adds 1g L-cysteine, 3g
Mass fraction is 20% ammoniacal liquor, 3g tetraethyl orthosilicates, continues to stir 5h at 35 DEG C, obtains reaction solution, and it is anti-that reaction solution is loaded into hydro-thermal
Answer in kettle, be heated to 170 DEG C of reaction 14h, be again heated to 220 DEG C of reaction 25h, be cooled to take out after room temperature and filter to obtain filter residue, use
Alternately washing to cleaning solution is in neutrality for deionized water and absolute ethyl alcohol, is placed in drying box, 4h is dried at 85 DEG C, obtains carbon materials
Material precursor, 1g carbon materials material precursors are taken, it is in 10% solution of potassium carbonate, with 350r/ at 75 DEG C to be immersed in 150g mass fractions
Min stirs 5h, filters to obtain filter cake, is washed with deionized to cleaning solution in neutrality, is placed in drying box, is dried at 85 DEG C
4h, it is reloaded into Muffle furnace, under nitrogen atmosphere, is heated to 550 DEG C of activated sintering 3h, after being cooled to room temperature, obtains molasses Ji Shui
Hot charcoal.
Example 3
20g molasses are taken, are added in 100mL deionized waters, 30min is stirred with 400r/min, adds 2g L-cysteine,
4g mass fractions are 20% ammoniacal liquor, 4g tetraethyl orthosilicates, continue to stir 6h at 40 DEG C, obtain reaction solution, reaction solution is loaded into hydro-thermal
In reactor, 180 DEG C of reaction 16h are heated to, are again heated to 240 DEG C of reaction 30h, is cooled to take out after room temperature and filters to obtain filter residue,
With deionized water and absolute ethyl alcohol, alternately washing to cleaning solution is in neutrality, is placed in drying box, 5h is dried at 90 DEG C, obtains carbon
Material precursor, take 2g carbon materials material precursors, be immersed in 200g mass fractions as in 10% solution of potassium carbonate, at 80 DEG C with
400r/min stirs 6h, filters to obtain filter cake, is washed with deionized to cleaning solution in neutrality, is placed in drying box, at 90 DEG C
5h is dried, is reloaded into Muffle furnace, under nitrogen atmosphere, is heated to 600 DEG C of activated sintering 4h, after being cooled to room temperature, obtains molasses
Base hydro-thermal charcoal.
Molasses base hydro-thermal charcoal prepared by the present invention and the hydro-thermal charcoal of Shandong company production are detected, specific detection knot
Fruit such as following table table 1：
The molasses base hydro-thermal charcoal performance characterization of table 1
The molasses base hydro-thermal charcoal that as shown in Table 1 prepared by the present invention, specific surface area increase, adsorbance increase, it is worth rate height, surface to be lived
Property enhancing, micropore distribution uniform, specific capacitance value is high, and stability is preferable.
Claims (6)
1. a kind of preparation method of molasses base hydro-thermal charcoal, it is characterised in that specifically preparation process is：
（1）After molasses are diluted with water and L-cysteine, mass fraction are 20% ammoniacal liquor, tetraethyl orthosilicate stirring reaction, are obtained
Reaction solution；
（2）Reaction solution is fitted into heating response in hydrothermal reaction kettle, is cooled to take out after room temperature and filters to obtain filter residue；
（3）Filter residue is alternately washed to cleaning solution in being dried after neutrality with deionized water and absolute ethyl alcohol, obtains carbon materials material precursor；
（4）Carbon materials material precursor is immersed in solution of potassium carbonate, 4~6h is stirred at 70~80 DEG C, filters to obtain filter cake；
（5）It will be fitted into after filter cake washing and drying in Muffle furnace, under nitrogen atmosphere, 3~4h of activated sintering, obtain molasses base hydro-thermal
Charcoal.
A kind of 2. preparation method of molasses base hydro-thermal charcoal as claimed in claim 1, it is characterised in that step（1）The molasses
Mass ratio with deionized water is 1：5.
A kind of 3. preparation method of molasses base hydro-thermal charcoal as claimed in claim 1, it is characterised in that step（1）The molasses,
L-cysteine, mass fraction are 20% ammoniacal liquor, the parts by weight of tetraethyl orthosilicate are 10 ~ 20 parts of molasses, the Guangs of 1~2 part of L-half
Propylhomoserin, 2~4 parts of mass fractions are 20% ammoniacal liquor, 2~4 parts of tetraethyl orthosilicates.
A kind of 4. preparation method of molasses base hydro-thermal charcoal as claimed in claim 1, it is characterised in that step（2）The heating
React to be heated to 160~180 DEG C of 12~16h of reaction, be again heated to 200~240 DEG C of 20~30h of reaction.
A kind of 5. preparation method of molasses base hydro-thermal charcoal as claimed in claim 1, it is characterised in that step（4）The carbonic acid
The mass fraction of potassium solution is 10%, and dosage is 50 ~ 200 times of carbon materials material precursor quality.
A kind of 6. preparation method of molasses base hydro-thermal charcoal as claimed in claim 1, it is characterised in that step（5）The activation
It is sintered to and is heated to 500~600 DEG C of 3~4h of activated sintering.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108520953A (en) * | 2018-04-17 | 2018-09-11 | 吉林大学 | A kind of carbon coating lithium titanate negative material and preparation method thereof |
| CN108638615A (en) * | 2018-04-19 | 2018-10-12 | 常州市蒽盗钟情生物科技有限公司 | A kind of preparation method of frog suit inner layer material |
| CN108816193A (en) * | 2018-06-14 | 2018-11-16 | 华南理工大学 | One kind having superelevation ultramicropore molasses base carbon material and the preparation method and application thereof |
| CN112169771A (en) * | 2020-09-17 | 2021-01-05 | 上海交通大学 | Preparation method of magnetic molasses hydrothermal carbon-based heavy metal adsorbent |
| CN113649044A (en) * | 2021-08-17 | 2021-11-16 | 温州大学 | Nitrogen-sulfur double-doped porous carbon material catalyst and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108520953A (en) * | 2018-04-17 | 2018-09-11 | 吉林大学 | A kind of carbon coating lithium titanate negative material and preparation method thereof |
| CN108638615A (en) * | 2018-04-19 | 2018-10-12 | 常州市蒽盗钟情生物科技有限公司 | A kind of preparation method of frog suit inner layer material |
| CN108816193A (en) * | 2018-06-14 | 2018-11-16 | 华南理工大学 | One kind having superelevation ultramicropore molasses base carbon material and the preparation method and application thereof |
| CN108816193B (en) * | 2018-06-14 | 2021-02-19 | 华南理工大学 | Molasses-based carbon material with ultrahigh ultramicropore and preparation method and application thereof |
| CN112169771A (en) * | 2020-09-17 | 2021-01-05 | 上海交通大学 | Preparation method of magnetic molasses hydrothermal carbon-based heavy metal adsorbent |
| CN113649044A (en) * | 2021-08-17 | 2021-11-16 | 温州大学 | Nitrogen-sulfur double-doped porous carbon material catalyst and preparation method thereof |
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Effective date of registration: 20180426 Address after: 213000 Tianhong science and technology building, 801 Changwu Middle Road, Wujin District, Changzhou, Jiangsu 416 Applicant after: Lei Chunsheng Address before: 213102 No. 6-205 Business Plaza, Nuo Cheng Gao Di, Tianning District, Changzhou, Jiangsu Applicant before: Changzhou Kay Textile Co., Ltd. |
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Application publication date: 20180316 |