CN107649100A - A kind of method that material for water treatment is prepared using lignin - Google Patents
A kind of method that material for water treatment is prepared using lignin Download PDFInfo
- Publication number
- CN107649100A CN107649100A CN201711098224.0A CN201711098224A CN107649100A CN 107649100 A CN107649100 A CN 107649100A CN 201711098224 A CN201711098224 A CN 201711098224A CN 107649100 A CN107649100 A CN 107649100A
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- Prior art keywords
- lignin
- prepared
- aeroge
- water treatment
- water
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention discloses a kind of method that material for water treatment is prepared using lignin, method is：Lignin is configured to the aqueous solution, lignin aeroge is obtained after freeze-dried, obtained lignin aeroge is placed in tube furnace in argon gas atmosphere and is heat-treated, described material for water treatment is obtained after cooling.After lignin presoma is crosslinked by the present invention by heat treatment method, it is prepared into the lignin-base material for water treatment of loose structure, the important functional group in lignin structure can not only be kept, it turn avoid its diffusion in water body, promote application of the lignin in water process, preparation method of the present invention is simple, and prepared material for water treatment is due to aerogel structure, important functional group in lignin structure is also retains simultaneously, thus there is preferable adsorption effect to pollutant.
Description
Technical field
The invention belongs to material for water treatment preparation field, and in particular to a kind of side that material for water treatment is prepared using lignin
Method.
Background technology
The improvement of water environment is the important topic of the world today, there is efficient adsorption capacity to pollutant, and cheap
Material for water treatment be always researcher exploitation important goal.
Containing functional groups such as substantial amounts of aromatic group, alkane hydroxyl, phenolic hydroxyl group, carboxyls in lignin structure, can directly inhale
Attached part heavy metal and organic pollution, and rich content of the lignin in nature, its content are only second to cellulose,
Lignin more discarded objects as paper-making industry in production and living are dropped at present, cause environmental pollution, therefore develop lignin
Value added applications, discarded lignin can be not only used, reduce the pollution to environment, and due to its price
Cheaply, source is unrestricted, receives significant attention in recent years.
But due to containing the water soluble groups such as hydroxyl, carboxyl in lignin structure, if directly as adsorption material
Material absorbs the pollutant in water body, then is difficult to play adsorption effect, and lignin can be made to be distributed in itself in water body environment, easily
Cause secondary pollution.
The content of the invention
For deficiencies of the prior art, water process is prepared using lignin it is an object of the invention to provide one kind
The method of material, when solving using lignin absorption pollutant, lignin is easily dispersed in water body environment and causes secondary pollution
Problem.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of method that material for water treatment is prepared using lignin, method are：It is 1 ~ 100mg/L's that lignin is configured into concentration
The aqueous solution, lignin aeroge is obtained after freeze-dried, obtained lignin aeroge is placed in tube furnace in argon gas gas
250 ~ 500 DEG C are heat-treated in atmosphere, and described material for water treatment is obtained after cooling.Wherein heat treatment temperature can be further excellent
Elect 300 ~ 350 DEG C as.
Preferably, the lignin concentration of aqueous solution is 1 ~ 10mg/L.Lignin concentration of aqueous solution is lower, aeroge
Density is also lower, and specific surface area can be bigger, and cross-linking effect is better during heat treatment, better to the adsorption effect of pollutant, still
Concentration is too low, and preparation efficiency and yield can decline.
Preferably, heat treatment time is 1 ~ 2h.
Preferably, the lignin is alkali lignin.
The lignin aqueous solution of the present invention can freeze in liquid nitrogen, can also use refrigerator freezing.Using liquid nitrogen frozen speed
It hurry up, the growth time of ice cube is short, and lignin is dispersed in smaller in ice cube, is advantageous to improve dried lignin airsetting
The intensity of glue.
Compared with prior art, the present invention has the advantages that：
1st, after lignin presoma is crosslinked by the present invention by heat treatment, it is prepared into the lignin-base water process material of loose structure
Material, can not only keep the important functional group in lignin structure, turn avoid its diffusion in water body, promote wooden
Application of the element in water process, wherein, the contact area between lignin molecule can be improved by freeze-drying, thus promote wood
The cross-linking effect of the intermolecular heat treatment of quality.
2nd, the present invention can be prepared at lignin-base water using discarded lignin by being freeze-dried and being heat-treated
Material is managed, preparation method is simple, and prepared material for water treatment also retains lignin knot due to aerogel structure
Important functional group in structure, thus there is preferable adsorption effect to pollutant.
3rd, the lignin aeroge of different densities is prepared by freeze-drying by the present invention, due to different concentration models
Enclose, the lignin pattern after freeze-drying is different, can regulate and control lignin presoma and friendship by adjusting lignin concentration of aqueous solution
The appearance structure of co-product, by adjusting heat treatment temperature, control the chemical composition of prepared material for water treatment.
4th, the inventive method need not use other cross-linking reagents or organic solvent, environmentally friendly and simple to operate
It is convenient, it is often more important that, the crosslinking lignin for being prepared by the method for the present invention out is therefore right due to there is larger specific surface area
Pollutant adsorption effect is more preferably.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of material for water treatment prepared by embodiment 1 ~ 4；
Fig. 2 is the infrared spectrogram of material for water treatment prepared by embodiment 4 ~ 7.
Embodiment
The present invention is described in further detail with reference to specific embodiment.
The lignin that following examples use is alkali lignin, and is conventionally configured to the aqueous solution.
Embodiment 1
By lignin dissolution in water, prepare the lignin aqueous solution of 100 mg/L concentration, by lignin liquor in liquid nitrogen it is fast
After quickly cooling is frozen, and it is freeze-dried, is prepared into lignin aeroge.Lignin aeroge is placed in tube furnace, in argon gas atmosphere
And be heat-treated 1 hour under the conditions of 300 DEG C, the microcosmic crosslinking lignin aeroge for sheet is prepared into after cooling, chemical composition contains
Free lignin, lignin portion crosslinking.
Wherein, product can be water-dispersible by infrared spectrum analysis, and by its, determines the ultraviolet spectra of scattered rear water
Figure, if ultraviolet have absorption, shows there is free lignin, the determination methods of following examples are so identical.
Embodiment 2
By lignin dissolution in water, prepare the lignin aqueous solution of 10 mg/L concentration, by lignin liquor in liquid nitrogen it is quick
After freezing, and it is freeze-dried, is prepared into lignin aeroge.Lignin aeroge is placed in tube furnace, in argon gas atmosphere and
It is heat-treated 1 hour under the conditions of 300 DEG C, the microcosmic crosslinking lignin aeroge for sheet is prepared into after cooling, chemical composition is containing trip
From lignin, lignin portion crosslinking.
Embodiment 3
By lignin dissolution in water, prepare the lignin aqueous solution of 5 mg/L concentration, by lignin liquor in liquid nitrogen it is quick
After freezing, and it is freeze-dried, is prepared into lignin aeroge.Lignin aeroge is placed in tube furnace, in argon gas atmosphere and
It is heat-treated 1 hour under the conditions of 300 DEG C, the microcosmic crosslinking lignin aeroge for sheet is prepared into after cooling, lignin is handed over substantially
Connection.
Embodiment 4
By lignin dissolution in water, prepare the lignin aqueous solution of 1 mg/L concentration, by lignin liquor in liquid nitrogen it is quick
After freezing, and it is freeze-dried, is prepared into lignin aeroge.Lignin aeroge is placed in tube furnace, in argon gas atmosphere and
It is heat-treated 1 hour under the conditions of 300 DEG C, the microcosmic crosslinking lignin aeroge for threadiness, the big portion of lignin is prepared into after cooling
Divide and crosslink.
Embodiment 5
By lignin dissolution in water, the lignin aqueous solution with 1 mg/L concentration, by lignin liquor in liquid nitrogen fast quickly cooling
After jelly, and it is freeze-dried, is prepared into lignin aeroge.Lignin aeroge is placed in tube furnace, in argon gas atmosphere and 350
It is heat-treated 1 hour under the conditions of DEG C, the microcosmic crosslinking lignin aeroge for threadiness is prepared into after cooling, lignin is largely sent out
Raw crosslinking.
Embodiment 6
By lignin dissolution in water, the lignin aqueous solution with 1 mg/L concentration, by lignin liquor in liquid nitrogen fast quickly cooling
After jelly, and it is freeze-dried, is prepared into lignin aeroge.Lignin aeroge is placed in tube furnace, in argon gas atmosphere and 400
It is heat-treated 1 hour under the conditions of DEG C, the microcosmic crosslinking lignin aeroge for threadiness, a small amount of carbon of lignin is prepared into after cooling
Change.
Embodiment 7
By lignin dissolution in water, the lignin aqueous solution with 1 mg/L concentration, by lignin liquor in liquid nitrogen fast quickly cooling
After jelly, and it is freeze-dried, is prepared into lignin aeroge.Lignin aeroge is placed in tube furnace, in argon gas atmosphere and 500
It is heat-treated 1 hour under the conditions of DEG C, the microcosmic crosslinking lignin aeroge for threadiness, lignin portion carbon is prepared into after cooling
Change.
Embodiment 8
By lignin dissolution in water, the lignin aqueous solution with 1 mg/L concentration, by lignin liquor in liquid nitrogen fast quickly cooling
After jelly, and it is freeze-dried, is prepared into lignin aeroge.Lignin aeroge is placed in tube furnace, in argon gas atmosphere and 250
It is heat-treated 1 hour under the conditions of DEG C, the microcosmic crosslinking lignin aeroge for sheet is prepared into after cooling, chemical composition is containing free
Lignin, lignin be not fully crosslinked.
In Fig. 1（1）、（2）、（3）、（4）The ESEM of material for water treatment respectively prepared by embodiment 1,2,3,4
Figure, as seen from Figure 1, with the reduction of freeze-drying lignin concentration, lignin pattern is turned by the sheet of very thick bulk
It is changed into the sheet of thin fritter, when lignin concentration is in below 5mg/mL, because lignin concentration is too low, it is in ice cube
Distribution can not support to form continuous laminated structure, be changed into threadiness from pellet module.
Fig. 2 is the infrared spectrogram of carbon material prepared by embodiment 4 ~ 7, as seen from the figure, when lignin is relatively
During such as 300,350 DEG C of low temperature, its chemical functional group such as phenolic hydroxyl group etc. can preserve well, when temperature further rises
Height, due to reasons such as the carbonizations of lignin material, its effective functional group gradually decreases.
Application test
It is respectively 10mg/L rhodamine B solution and 30mg/L copper ion solution to prepare initial concentration, and it is real to use it for test
Apply the absorption property of crosslinking lignin aeroge prepared by example 4 and embodiment 5.
Method of testing is：The crosslinking lignin aeroge of preparation is dispersed in pending solution, is placed on and shakes
Swing and absorption 12h is rocked on device, then reclaim crosslinking lignin aeroge therein, and determine rhodamine B or copper ion in solution
Concentration.
Test result shows：Crosslinking lignin aeroge prepared by embodiment 4 is reachable to the adsorption capacity of rhodamine B
157mg/g, to the adsorption capacity of copper ion solution up to 290mg/g；Crosslinking lignin aeroge prepared by embodiment 5 is to Luo Dan
Bright B solution and the adsorption capacity of copper ion solution respectively reach 47mg/g and 340mg/g.
The above embodiment of the present invention is only example to illustrate the invention, and is not the implementation to the present invention
The restriction of mode.For those of ordinary skill in the field, other can also be made not on the basis of the above description
With the change and variation of form.Here all embodiments can not be exhaustive.It is every to belong to technical scheme
Row of the obvious changes or variations amplified out still in protection scope of the present invention.
Claims (4)
- A kind of 1. method that material for water treatment is prepared using lignin, it is characterised in that by lignin be configured to concentration for 1 ~ The 100mg/L aqueous solution, lignin aeroge is obtained after freeze-dried, obtained lignin aeroge is placed in tube furnace 250 ~ 500 DEG C are heat-treated in argon gas atmosphere, and described material for water treatment is obtained after cooling.
- 2. the method according to claim 1 that material for water treatment is prepared using lignin, it is characterised in that the lignin Concentration of aqueous solution is 1 ~ 10mg/L.
- 3. the method according to claim 1 that material for water treatment is prepared using lignin, it is characterised in that heat treatment time For 1 ~ 2h.
- 4. the method according to claim 1 that material for water treatment is prepared using lignin, it is characterised in that the lignin For alkali lignin.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711098224.0A CN107649100B (en) | 2017-11-09 | 2017-11-09 | Method for preparing water treatment material by using lignin |
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| CN201711098224.0A CN107649100B (en) | 2017-11-09 | 2017-11-09 | Method for preparing water treatment material by using lignin |
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| CN107649100A true CN107649100A (en) | 2018-02-02 |
| CN107649100B CN107649100B (en) | 2020-06-02 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108704619A (en) * | 2018-06-07 | 2018-10-26 | 石梦成 | A kind of magnetism lignin aeroge waste water treating agent and preparation method thereof |
| CN109292760A (en) * | 2018-11-30 | 2019-02-01 | 长江师范学院 | A method of preparing graphene |
| CN116159549A (en) * | 2023-04-26 | 2023-05-26 | 西安博探石油工程有限公司 | Hydrogen sulfide gas adsorption material and preparation method and application thereof |
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Cited By (3)
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|---|---|---|---|---|
| CN108704619A (en) * | 2018-06-07 | 2018-10-26 | 石梦成 | A kind of magnetism lignin aeroge waste water treating agent and preparation method thereof |
| CN109292760A (en) * | 2018-11-30 | 2019-02-01 | 长江师范学院 | A method of preparing graphene |
| CN116159549A (en) * | 2023-04-26 | 2023-05-26 | 西安博探石油工程有限公司 | Hydrogen sulfide gas adsorption material and preparation method and application thereof |
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