CN106350064A - Method to prepare water-soluble fluorescent carbon material by carbonizing papermaking black liquor by microwave heating - Google Patents
Method to prepare water-soluble fluorescent carbon material by carbonizing papermaking black liquor by microwave heating Download PDFInfo
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- CN106350064A CN106350064A CN201610761060.4A CN201610761060A CN106350064A CN 106350064 A CN106350064 A CN 106350064A CN 201610761060 A CN201610761060 A CN 201610761060A CN 106350064 A CN106350064 A CN 106350064A
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- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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Abstract
The invention discloses a method to prepare water-soluble fluorescent carbon material by carbonizing papermaking black liquor by microwave heating. The method to prepare carbon material by hydrothermal cabonization, as the environment friendly treatment method of high polymer organic matter that emerges in recent years, the cost is low, the reaction conditions are relatively mild, and new type of carbon material with good water solubility and rich functional group on the surface can be obtained. The invention takes paper making black liquor as the raw material. In the microwave high pressure reactor, perform hydrothermal carbonization reaction by microwave heating at 180-250oC for 1-6h. After the reaction, perform suction filtration for the products with a funnel with the hole diameter of 1.5-2.5Mum to obtain brownish black solution. Then pour the brownish black solution into a dialysis bag with the molecular weight of at least 3,500 for dialysis, and water-soluble fluorescent carbon material is left in the dialysis bag. At the carbon spot, the solution has steep absorption peak at 225nm, and relatively weak UV absorption peak at 350nm. Freeze dry the water-soluble carbon material in the dialysis bag to obtain yellow solid carbon material powder with the particle diameter of about 10nm.
Description
Technical field
The present invention relates to a kind of method preparing water soluble fluorescence material with carbon element, more particularly to one kind utilize black liquid system
The method of standby water soluble fluorescence material with carbon element, is applied to sewage disposal and changing rejected material to useful resource technical field.
Background technology
In recent years, the paper waste produced pollution is only second to metallurgy, petrochemical industry occupies the 3rd, and discharge capacity accounts for whole industry
Black liquor produced by the 1/6 of wastewater discharge, wherein pulping process accounts for the 90% of total paper waste, if not carrying out processing directly
Discharge will heavy damage ecological environment.
In black liquid, contained main component is lignin and its catabolite.Lignin is by guaiacyl, purple fourth
Perfume base and p-hydroxyphenyl construction unit composition macromolecular compound.Due to its complicated structure, limit its industrialized utilization.Have
Material with carbon element is prepared in the hydro-thermal carbonization of machine matter, and reaction condition is gentle, less energy intensive, and it is to carry out in aqueous, need not be to former
Material carries out the dried of early stage, it is to avoid the problem of environmental pollution that organic solvent brings, is a kind of friendly process process.But by
In hydro-thermal carbonization temperature many below 350 DEG C, compare at least 600 DEG C high temperature above of relatively straightforward high temperature pyrolysis process, temperature
Very low, carbonization efficiency comparison is low.
Content of the invention
In order to solve prior art problem, it is an object of the invention to overcoming the shortcomings of that prior art exists, provide one kind
The method preparing water soluble fluorescence material with carbon element using microwave heating method hydro-thermal carbonization black liquid, using microwave heating hydro-thermal carbonization
Method, the organic pollution that key component in black liquid is lignin is converted into the water-soluble fluorescent carbon of high added value
Material, eliminates paper-making black liquor, realizes environment and economical effects.The present invention is made by microwave heating Direct Hydrothermal carbonization
Paper black liquor, it is not necessary to catalyst, can prepare water miscible fluorescence material with carbon element, process is simple, have efficiently, environmental protection, green
The features such as.
Create purpose for reaching foregoing invention, the present invention is using following inventive concepts:
Effect by outfield is improved the practical application being undoubtedly conducive to hydro-thermal charring, and microwave is that frequency about exists
Electromagnetic wave in the range of 300mhz～300ghz, compared to traditional mode of heating, microwave technology is promoting chemical reaction course
There is the advantage of uniqueness with the selectivity aspect of response speed and product etc..Under this heating condition, in addition to heat effect, micro-
Wave field frequency change can lead to reactant molecule to reach dynamic balance state by moving or rotating generation torque, causes molecule to transport
Move and certain orientation is had on microcosmic, improve effective collision probability, thus accelerating chemical reaction rate, improving reaction yield and selection
Property.Therefore, hydro-thermal carbonization process can be strengthened using microwave heating, be conducive to preparing water soluble fluorescence using carbonization black liquid
The realization of material with carbon element technique.
Conceived according to foregoing invention, the present invention adopts following technical proposals:
A kind of method preparing water soluble fluorescence material with carbon element using microwave heating method hydro-thermal carbonization black liquid, walks including following
Rapid:
A. hydro-thermal charring process: black liquid is added in microwave reaction kettle, carries out 1-6h at temperature is for 180-250 DEG C
Response time in carry out hydro-thermal carbonization reaction；As currently preferred technical scheme, carry out at temperature is for 220-240 DEG C
Carry out hydro-thermal carbonization reaction in the response time of 3-4h；
B. the separation of water soluble fluorescence material with carbon element: after the hydro-thermal carbonization reaction in described step a terminates, question response kettle is natural
After being cooled to room temperature, then product takes out from reactor after reacting, and then using aperture, the funnel for 1.5-2.5 μm is taken out
Filter, obtains dark brown solution, and the bag filter subsequently pouring this dark brown solution into molecular cut off at least 3500 is dialysed,
The solution obtaining in bag filter afterwards, as has the water solublity carbon dots solution of fluorescent characteristic；Preferably use g5 sand core funnel pair
Product carries out sucking filtration；
C. water soluble fluorescence material with carbon element collect: by described step b in bag filter gained water solublity carbon dots solution lyophilizing
Afterwards, yellow solid carbon material powder, as water soluble fluorescence material with carbon element are obtained.
The present invention compared with prior art, has and obviously projects substantive distinguishing features and remarkable advantage as follows:
1. the method that the present invention enhances hydro-thermal carbonization using microwave heating, key component in black liquid is lignin
Organic pollution, be converted into the water soluble fluorescence material with carbon element of high added value, solve paper-making black liquor, realize environment with economical
Double benefit；
2. hydro-thermal carbonization of the present invention prepares material with carbon element as the organic process side of the macromolecule of the environmental protection occurring in recent years
Method, with low cost, reaction condition is relatively mild, can get the new carbon that there is the good aqueous solubility of abundant functional group on surface.
Brief description
Fig. 1 is the UV-visible spectrum of the water solublity carbon dots solution of the embodiment of the present invention one preparation.
Fig. 2 is transmission electron microscope (tem) image of the water soluble fluorescence material with carbon element of the embodiment of the present invention one preparation.
Specific embodiment
Details are as follows for the preferred embodiments of the present invention:
Embodiment one:
In the present embodiment, referring to Fig. 1 and Fig. 2, it is glimmering that one kind prepares water solublity using microwave heating method hydro-thermal carbonization black liquid
The method of light material with carbon element, comprises the steps:
A. hydro-thermal charring process: the 300ml black liquid black liquid containing lignin 30% is added in microwave reaction kettle, if
Put temperature and be 240 DEG C, carry out the hydro-thermal carbonization reaction of 3h at this temperature；
B. the separation of water soluble fluorescence material with carbon element: after the hydro-thermal carbonization reaction in described step a terminates, question response kettle is natural
After being cooled to room temperature, then product takes out from reactor after reacting, the then g5 sand core funnel for 1.5-2.5 μm using aperture
Carry out sucking filtration, obtain dark brown solution, subsequently pour this dark brown solution into bag filter that molecular cut off is 3500 and dialysed,
The last solution obtaining in bag filter, as has the water solublity carbon dots solution of fluorescent characteristic；
C. water soluble fluorescence material with carbon element collect: by described step b in bag filter gained water solublity carbon dots solution lyophilizing
Afterwards, yellow solid carbon material powder, as water soluble fluorescence material with carbon element are obtained.
Experimental test and analysis:
The water soluble fluorescence material with carbon element of the water solublity carbon dots solution to the step b preparation of the present embodiment and the preparation of step c enters respectively
Row experimental test and analysis.The UV-visible spectrum of the water solublity carbon dots solution that Fig. 1 is prepared for step b, except at 225nm
Have outside precipitous absworption peak, ultraviolet characteristic absorption peak also relatively weak at 350nm.Fig. 2 is to be 3500 through molecular weight
After bag filter dialysis, transmission electron microscope (tem) image of gained yellow solid carbon point powder, i.e. step after solution lyophilizing in bag filter
The water-soluble fluorescent carbon material transmission sem image of c preparation.Its particle diameter is close to 10nm as seen from Figure 2.Prepared by the present embodiment
The aqueous solution of water soluble fluorescence material with carbon element place at ambient temperature 1 week, there is no any obvious sedimentation, show steady for a long time
Fixed is homogeneous.The aqueous solution of water soluble fluorescence material with carbon element manufactured in the present embodiment Continuous irradiation 30min under 365nm exciting light,
Fluorescence intensity is almost unchanged, shows that it has excellent anti-light Bleachability, is conducive to carbon point in the side such as cell-targeting spike, imaging
The application in face.Additionally, the aqueous solution of water soluble fluorescence material with carbon element manufactured in the present embodiment is in the sodium chloride concentration scope of 0-2.0m
Interior, fluorescence intensity is also basicly stable constant, illustrates there is good saline-alkaline tolerance, is conducive to it in terms of biochemical analysis and detection
Application.
Because lignin is the main component of black liquid, directly discharge can cause very big destruction to environment.This enforcement
Example hydro-thermal carbonization prepares material with carbon element as the organic processing method of the macromolecule of the environmental protection occurring in recent years, low cost
Honest and clean, reaction condition is relatively mild, can get the new carbon that there is the good aqueous solubility of abundant functional group on surface.This patent is to make
Paper black liquor is raw material, in microwave high pressure reactor, by microwave heating, carries out hydro-thermal carbonization reaction, product after the completion of reaction
Carry out sucking filtration using g5 sand core funnel, obtain dark brown solution.Subsequently pouring this dark brown solution into molecular cut off is 3500
Bag filter is dialysed, and has obtained water miscible fluorescence material with carbon element in bag filter.This carbon dots solution is precipitous except having at 225nm
Absworption peak outside, ultraviolet characteristic absorption peak also relatively weak at 350nm.Water soluble fluorescence carbon materials by gained in bag filter
Material lyophilizing after, obtain particle diameter about 10nm about yellow solid carbon material powder.The present embodiment is in the condition of microwave heating
Under, main Organic substance lignin carbonization in black liquor obtains water miscible fluorescence material with carbon element, by key component in black liquid
For the organic pollution of lignin, it is converted into the water soluble fluorescence material with carbon element of high added value, solves paper-making black liquor, realize
Environment and economical effects.
Embodiment two:
The present embodiment is essentially identical with embodiment one, is particular in that:
In the present embodiment, a kind of side preparing water soluble fluorescence material with carbon element using microwave heating method hydro-thermal carbonization black liquid
Method, comprises the steps:
A. hydro-thermal charring process: the 300ml black liquid black liquid containing lignin 30% is added in microwave reaction kettle, if
Put temperature and be 220 DEG C, carry out the hydro-thermal carbonization reaction of 4h at this temperature；
B. this step is identical with embodiment one；
C. this step is identical with embodiment one.
Experimental test and analysis:
Experimental test and analysis are carried out to water soluble fluorescence material with carbon element manufactured in the present embodiment.Water soluble fluorescence manufactured in the present embodiment
The aqueous solution of material with carbon element is placed 1 week at ambient temperature, does not have any obvious sedimentation, shows steady in a long-term homogeneous.This
The aqueous solution of the water soluble fluorescence material with carbon element of embodiment preparation Continuous irradiation 30min under 365nm exciting light, fluorescence intensity is almost
Constant, show that it has excellent anti-light Bleachability, be conducive to carbon point in the application of the aspects such as cell-targeting spike, imaging.This
Outward, the aqueous solution of water soluble fluorescence material with carbon element manufactured in the present embodiment is in the range of the sodium chloride concentration of 0-2.0m, fluorescence intensity
Also basicly stable constant, illustrate that there is good saline-alkaline tolerance, be conducive to its application in terms of biochemical analysis and detection.
Embodiment three:
The present embodiment is substantially the same as in the previous example, and is particular in that:
In the present embodiment, a kind of side preparing water soluble fluorescence material with carbon element using microwave heating method hydro-thermal carbonization black liquid
Method, comprises the steps:
A. hydro-thermal charring process: the 300ml black liquid black liquid containing lignin 30% is added in microwave reaction kettle, if
Put temperature and be 180 DEG C, carry out the hydro-thermal carbonization reaction of 6h at this temperature；
B. this step is identical with embodiment one；
C. this step is identical with embodiment one.
The efficiency of water soluble fluorescence material with carbon element manufactured in the present embodiment compare embodiment low some, but due to the present embodiment
The method employing assisted microwave synthesis heating, still above traditional direct high temperature pyrolysis process carries out hydro-thermal carbonization reaction preparation
The efficiency of fluorescence material with carbon element, so the present embodiment still achieves the purpose of the present invention.
Example IV:
The present embodiment is substantially the same as in the previous example, and is particular in that:
In the present embodiment, a kind of side preparing water soluble fluorescence material with carbon element using microwave heating method hydro-thermal carbonization black liquid
Method, comprises the steps:
A. hydro-thermal charring process: the 300ml black liquid black liquid containing lignin 30% is added in microwave reaction kettle, if
Put temperature and be 250 DEG C, carry out the hydro-thermal carbonization reaction of 1h at this temperature；
B. this step is identical with embodiment one；
C. this step is identical with embodiment one.
The efficiency of water soluble fluorescence material with carbon element manufactured in the present embodiment compare embodiment low some, but due to the present embodiment
The method employing assisted microwave synthesis heating, still above traditional direct high temperature pyrolysis process carries out hydro-thermal carbonization reaction preparation
The efficiency of fluorescence material with carbon element, so the present embodiment still achieves the purpose of the present invention.
Above in conjunction with accompanying drawing, the embodiment of the present invention is illustrated, but the invention is not restricted to above-described embodiment, acceptable
The purpose of the innovation and creation according to the present invention makes multiple changes, under all spirit and principle according to technical solution of the present invention
Change, modification, replacement, combination or the simplification made, all should be equivalent substitute mode, as long as meeting the goal of the invention of the present invention,
Prepare the skill of the method for water soluble fluorescence material with carbon element without departing from the present invention using microwave heating method hydro-thermal carbonization black liquid
Art principle and inventive concept, broadly fall into protection scope of the present invention.
Claims (3)
1. a kind of method preparing water soluble fluorescence material with carbon element using microwave heating method hydro-thermal carbonization black liquid, its feature exists
In comprising the steps:
A. hydro-thermal charring process: black liquid is added in microwave reaction kettle, carries out 1-6h at temperature is for 180-250 DEG C
Response time in carry out hydro-thermal carbonization reaction；
B. the separation of water soluble fluorescence material with carbon element: after the hydro-thermal carbonization reaction in described step a terminates, question response kettle is natural
After being cooled to room temperature, then product takes out from reactor after reacting, and then using aperture, the funnel for 1.5-2.5 μm is taken out
Filter, obtains dark brown solution, and the bag filter subsequently pouring this dark brown solution into molecular cut off at least 3500 is dialysed,
The solution obtaining in bag filter afterwards, as has the water solublity carbon dots solution of fluorescent characteristic；
C. water soluble fluorescence material with carbon element collect: by described step b in bag filter gained water solublity carbon dots solution lyophilizing
Afterwards, yellow solid carbon material powder, as water soluble fluorescence material with carbon element are obtained.
2. the side of water soluble fluorescence material with carbon element is prepared according to claim 1 using microwave heating method hydro-thermal carbonization black liquid
Method it is characterised in that: in described step a, in response time of carrying out 3-4h at temperature is for 220-240 DEG C, carry out hydro-thermal charcoal
Change reaction.
3. according to claim 1 or claim 2 prepare water soluble fluorescence material with carbon element using microwave heating method hydro-thermal carbonization black liquid
Method it is characterised in that: in described step b, using g5 sand core funnel, sucking filtration is carried out to product.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110255523A (en) * | 2018-03-12 | 2019-09-20 | 天津大学 | A kind of preparation method of carbon-based photothermal conversion film |
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| CN110255523A (en) * | 2018-03-12 | 2019-09-20 | 天津大学 | A kind of preparation method of carbon-based photothermal conversion film |
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