CN109999757A - A kind of Cr-MOF/ wood composite aeroge and preparation method and application capturing heavy metal ion - Google Patents
A kind of Cr-MOF/ wood composite aeroge and preparation method and application capturing heavy metal ion Download PDFInfo
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- CN109999757A CN109999757A CN201910305848.8A CN201910305848A CN109999757A CN 109999757 A CN109999757 A CN 109999757A CN 201910305848 A CN201910305848 A CN 201910305848A CN 109999757 A CN109999757 A CN 109999757A
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- 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
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
- B01J20/226—Coordination polymers, e.g. metal-organic frameworks [MOF], zeolitic imidazolate frameworks [ZIF]
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
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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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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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
- C02F2101/00—Nature of the contaminant
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Abstract
The invention belongs to technical field of composite materials, provide a kind of preparation method of Cr-MOF/ wood composite aeroge that can capture heavy metal ion, include the following steps: step S1, desiccated wood is prepared into timber hydrogel；Step S2, the timber hydrogel is immersed and carries out hydro-thermal reaction in sealing reactor containing the solution that can form Cr-MOF, form Cr-MOF/ wood composite hydrogel；Step S3, the Cr-MOF/ wood composite hydrogel is dried, obtains Cr-MOF/ wood composite aeroge.The preparation method of the Cr-MOF/ wood composite aeroge for capturing heavy metal ion of the invention, Cr-MOF is combined with timber hydrogel by hydro-thermal method, being formed has the Cr-MOF/ wood composite aeroge for capturing heavy metal ion function, simple process and reacts at low temperature, easy to operate.
Description
Technical field
The present invention relates to technical field of composite materials, and in particular to one kind can capture the Cr-MOF/ timber of heavy metal ion
Composite aerogel and preparation method and application.
Background technique
In recent years, with the fast development of economic construction of China, the exploitation of heavy metal, smelting, processing and business are manufactured
Activity is increasing, and many heavy metals (such as lead, caesium, strontium) is caused to enter big gas and water, in soil, has caused a series of serious
Contamination accident, great harm is caused to ecological environment.Acute poisoning caused by heavy metal and each anthropoid chronic disease
Such as senile dementia, also the moment threatens the health of the mankind.Some heavy metal ion will be to biology in very low concentrations
Body has extremely strong toxicity, and different from organic compound, and heavy metal has enriching, is difficult to be degraded in the natural environment.
Due to the limitation of production technology, a large amount of weight is contained in waste, such as industrial wastewater caused by a series of production activities
Metal ion, this can both damage ecological environment, but also production cost is high.
These materials to heavy metal ions in sewage with capture function developed at present are mostly inanimate matter material, and
It is single that there are adsorption functions, and capture amount is small and dynamics is slow, and deposition process generally requires to carry out several hundred hours.
Summary of the invention
For the defects in the prior art, the present invention provides a kind of Cr-MOF/ wood composite that can capture heavy metal ion
Aeroge, with solve the problems, such as how efficiently and while capturing contents of many kinds of heavy metal ion.
In a first aspect, the preparation side of the Cr-MOF/ wood composite aeroge provided by the invention for capturing heavy metal ion
Method includes the following steps:
Step S1, desiccated wood is prepared into timber hydrogel；
Step S2, the timber hydrogel is immersed and carries out water in sealing reactor containing the solution that can form Cr-MOF
Thermal response forms Cr-MOF/ wood composite hydrogel；
Step S3, the Cr-MOF/ wood composite hydrogel is dried, obtains the airsetting of Cr-MOF/ wood composite
Glue.
Optionally, specific step is as follows by the step S1:
By the desiccated wood, successively acidified oxidant carries out acidification and lye carries out basification.
Optionally, the moisture content of the desiccated wood in the step S1 is 0.1%~30%, the type of the desiccated wood
For poplar, birch, China fir or cork wood.
Optionally, the acidification oxidant be hydrogen oxide, it is Peracetic acid, sodium dichromate, ammonium persulfate, sodium chlorite, secondary
The pH of sodium chlorate, SODIUM PERCARBONATE, sodium perborate or potassium perborate, the acidification oxidant is 1.0~6.0, the acidification oxidation
The mass percent of agent is 0.1%~30%；
The temperature of the acidification is 20~100 DEG C, and the processing time is 1~120 hour.
Optionally, the lye is lithium hydroxide, sodium hydroxide, potassium hydroxide or ammonium hydroxide, the quality percentage of the lye
Than being 1%~20%；
The temperature of the basification is 20~100 DEG C, and the processing time is 1~120 hour.
Optionally, can be formed described in the step S2 Cr-MOF solution include molar ratio be 1:1:2 nine water nitric acid
Chromium, 2- amino terephthalic acid (TPA) and sodium hydroxide.
Optionally, the temperature that hydro-thermal reaction is carried out in the step S2 is 50~200 DEG C, and the processing time is 1~120 small
When.
Optionally, the mode of the drying process in the step S3 is vacuum freeze drying, critical point drying or overcritical
It is dry.
Second aspect, the present invention provide the Cr-MOF/ wood composite aeroge that can capture heavy metal ion as mentioned
Cr-MOF/ wood composite aeroge prepared by preparation method.
The third aspect, the present invention provide Cr-MOF/ wood composite aeroge as mentioned and are capturing heavy metal from sewage
The application of ion.
Beneficial effects of the present invention:
1. the preparation method of the Cr-MOF/ wood composite aeroge for capturing heavy metal ion of the invention, passes through hydro-thermal
Method combines Cr-MOF with timber hydrogel, and being formed has the Cr-MOF/ wood composite airsetting for capturing heavy metal ion function
Glue, simple process and reacts at low temperature, easy to operate.
2. the Cr-MOF/ wood composite aeroge prepared by the present invention for capturing heavy metal ion has good three-dimensional
Layer structure can effectively capture heavy metal ion, be a kind of novel heavy metal ion capture function material.
3. the Cr-MOF/ wood composite aeroge for capturing heavy metal ion of the invention, shows powerful in sewage
Balance capture ability, to Pb2+Maximum capture capacity be 3.64mmol/g, to Sr2+Maximum capture capacity be
1.61mmol/g, to CS+Maximum capture capacity be 0.41mmol/g.
Detailed description of the invention
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art are briefly described.In all the appended drawings, similar element
Or part is generally identified by similar appended drawing reference.In attached drawing, each element or part might not be drawn according to actual ratio.
Fig. 1 is the XRD test chart of Cr-MOF/ wood composite aeroge provided by the embodiment of the present invention 1；
Fig. 2 is the SEM figure of Cr-MOF/ wood composite aeroge provided by the embodiment of the present invention 1；
Fig. 3 is to capture Pb2+The XPS figure of Cr-MOF/ wood composite aeroge afterwards；
Fig. 4 is that Cr-MOF/ wood composite aeroge captures Pb2+Dynamic Adsorption curve；
Fig. 5 is that Cr-MOF/ wood composite aeroge captures Sr2+Dynamic Adsorption curve；
Fig. 6 is that Cr-MOF/ wood composite aeroge captures CS+Dynamic Adsorption curve.
Specific embodiment
It is described in detail below in conjunction with embodiment of the attached drawing to technical solution of the present invention.Following embodiment is only used for
Clearly illustrate technical solution of the present invention, therefore be intended only as example, and cannot be used as a limitation and limit protection of the invention
Range.
It should be noted that unless otherwise indicated, technical term or scientific term used in this application should be this hair
The ordinary meaning that bright one of ordinary skill in the art are understood.
The present invention provides the preparation methods for the Cr-MOF/ wood composite aeroge that can capture heavy metal ion, including such as
Lower step:
Step S1, by desiccated wood, successively acidified oxidant carries out acidification and lye carries out basification, preparation
At timber hydrogel；
Wherein, the moisture content of desiccated wood is 0.1%~30%, and the type of the desiccated wood is poplar, birch, China fir
Or cork wood.
The acidification oxidant be hydrogen oxide, Peracetic acid, sodium dichromate, ammonium persulfate, sodium chlorite, sodium hypochlorite,
The pH of SODIUM PERCARBONATE, sodium perborate or potassium perborate, the acidification oxidant is 1.0~6.0, the quality of the acidification oxidant
Percentage is 0.1%~30%；
The temperature of the acidification is 20~100 DEG C, and the processing time is 1~120 hour.
The lye is lithium hydroxide, sodium hydroxide, potassium hydroxide or ammonium hydroxide, and the mass percent of the lye is 1%
~20%；
The temperature of the basification is 20~100 DEG C, and the processing time is 1~120 hour.
Timber mainly by cellulose, hemicellulose and lignin composition, first carries out acidification, removes wooden in timber
Plain component, then basification is carried out, the hemicellulose in timber is removed, cellulose timber hydrogel is finally obtained.
Step S2, the timber hydrogel is immersed and carries out water in sealing reactor containing the solution that can form Cr-MOF
Thermal response forms Cr-MOF/ wood composite hydrogel, wherein it is 1:1:2 that the solution that can form Cr-MOF, which includes molar ratio,
Nine water chromic nitrates, 2- amino terephthalic acid (TPA) and sodium hydroxide；
The temperature of hydro-thermal reaction is 50~200 DEG C, and the processing time is 1~120 hour.
When timber hydrogel is immersed in containing in the solution that can form Cr-MOF, Cr3+Wood is incorporated in by the effect of hydrogen bond
In material hydrogel, in the high temperature that hydro-thermal reaction provides, Cr3+Ion and 2- amino terephthalic acid (TPA) occur instead under alkaline condition
It answers, generates Cr-MOF；By after a few hours, Cr-MOF is acted in timber hydrogel by hydrogen bond and electrostatic attraction
Even growth.
Step S3, the Cr-MOF/ wood composite hydrogel is dried, obtains the airsetting of Cr-MOF/ wood composite
Glue, wherein the mode of drying process is vacuum freeze drying, critical point drying or supercritical drying.
For preparation method of the invention, the present invention also provides embodiment 1-3.
Embodiment 1
1. being successively 4.2 in pH by the cork wood for being 8% having a size of 10mm x10mm x10mm, moisture content, mass fraction is
80 DEG C of acidifications 6 hours, 95 DEG C of basifications of sodium hydroxide solution that mass fraction is 10% in 1% sodium chlorite solution
6 hours, timber hydrogel was obtained after timber washs 3 times in the solution of alcohol water by treated；
2. timber hydrogel is put into nine water chromic nitrates, 2- amino terephthalic acid (TPA) and the hydroxide that molar ratio is 1:1:2
In the solution of sodium, then hydro-thermal reaction 10 hours at 150 DEG C, Cr-MOF/ wood composite hydrogel is obtained；
3. claiming Cr-MOF/ wood composite aeroge can be obtained after the freeze-drying of Cr-MOF/ wood composite hydrogel
Weight obtains 80mgCr-MOF/ wood composite aeroge.
Fig. 1 is the XRD diagram of Cr-MOF/ wood composite aeroge provided by the embodiment of the present invention 1.As shown in Figure 1,2 θ values
The crystal region of cellulose in timber hydrogel is attributed to for the diffraction maximum of 16 ° and 22 °.In addition, other characteristic peaks belong to Cr-
MOF.After timber hydrogel and Cr-MOF combine, the characteristic peak of cellulose and Cr-MOF are retained in Cr-MOF/ wood composite gas
In the XRD diagram of gel.These results indicate that Cr-MOF/ wood composite aeroge successfully synthesizes.
Fig. 2 is the SEM figure of Cr-MOF/ wood composite aeroge provided by the embodiment of the present invention 1.As shown in Fig. 2, by
Acidified sodium chlorite and sodium hydroxide solution processing to cork wood, observe that Cr-MOF/ wood composite aeroge possesses stratiform knot
Structure illustrates to eliminate hemicellulose and lignin.Cr3+The effect for first passing through hydrogen bond is incorporated in timber hydrogel.Later, exist
In 150 DEG C of heat treatment processes, Cr3+It reacts under alkaline condition with 2- amino terephthalic acid (TPA), octahedra Cr-MOF is in layer
It is grown in shape timber hydrogel, Cr-MOF/ wood composite aeroge successfully synthesizes.
Embodiment 2
1. being successively 3.0 in pH by the poplar for being 1% having a size of 10mm x10mm x10mm, moisture content, mass fraction is
70 DEG C of acidifications 10 hours in 5% sodium chlorite solution, at 90 DEG C of alkalization of sodium hydroxide solution that mass fraction is 12%
Reason 10 hours obtains timber hydrogel after timber washs 3 times in the solution of alcohol water for treated；
2. timber hydrogel is put into nine water chromic nitrates, 2- amino terephthalic acid (TPA) and the hydroxide that molar ratio is 1:1:2
In the solution of sodium, then hydro-thermal reaction 12 hours at 120 DEG C, Cr-MOF/ wood composite hydrogel is obtained；
3. claiming Cr-MOF/ wood composite aeroge can be obtained after Cr-MOF/ wood composite hydrogel critical point drying
Weight obtains 78mgCr-MOF/ wood composite aeroge.
Embodiment 3
1. being successively 5.0 in pH by the China fir for being 10% having a size of 10mm x10mm x10mm, moisture content, mass fraction is
85 DEG C of acidifications 8 hours, 90 DEG C of basifications of sodium hydroxide solution that mass fraction is 10% in 8% sodium chlorite solution
12 hours, timber hydrogel was obtained after timber washs 3 times in the solution of alcohol water by treated；
2. timber hydrogel is put into nine water chromic nitrates, 2- amino terephthalic acid (TPA) and the hydroxide that molar ratio is 1:1:2
In the solution of sodium, then hydro-thermal reaction 6 hours at 180 DEG C, Cr-MOF/ wood composite hydrogel is obtained；
3. claiming Cr-MOF/ wood composite aeroge can be obtained after the freeze-drying of Cr-MOF/ wood composite hydrogel
Weight obtains 77mgCr-MOF/ wood composite aeroge.
Embodiment 4
Can the Cr-MOF/ wood composite aeroge that the present embodiment is prepared for embodiment 2 adsorb heavy metal ion progress
Verification experimental verification.
Cr-MOF/ wood composite aeroge prepared by embodiment 2 is put into the Pb for being only 8mmol/L containing concentration2+'s
In solution, to Pb in solution2+Concentration constantly reduce, until be no longer changed, take out Cr-MOF/ wood composite gas therein
Gel, and XPS analysis is carried out to it.Fig. 3 is to capture Pb2+The XPS figure of Cr-MOF/ wood composite aeroge afterwards.As seen from Figure 3,
Adsorb Pb2+Cr-MOF/ wood composite aeroge is mainly by Cr, O, N, C and Pb element composition afterwards.Cr 2P, O 1s, N 1s and C
1s belongs to Cr-MOF/ wood composite aeroge, and wherein N belongs to the-NH2 functional group for grafting on Cr-MOF.The peak Pb 4f goes out
It is existing, illustrate that Cr-MOF/ wood composite aeroge successfully captures heavy metal ion Pb2+。
Embodiment 5
The present embodiment is directed to the Cr-MOF/ wood composite aeroge of the preparation of embodiment 1 to a huge sum of money using dynamic adsorption test
The adsorption capacity for belonging to ion is tested.
Test is carried out at 20 DEG C.100mL testing liquid is prepared before test in advance, it is equal to contain initial concentration in testing liquid
For the Pb of 8mmol/L2+、Sr2+And Cs+.80mgCr-MOF/ wood composite aeroge is put into testing liquid, and every one
It fixes time and detects Pb in testing liquid2+、Sr2+And Cs+Ion concentration, and record.
Pb is calculated as follows2+、Sr2+And Cs+Capture capacity.
Capture capacity
Wherein, C0(mmol·L-1) be ion initial concentration；Ce(mmol·L-1) be ion equilibrium concentration；M be from
The relative atomic mass of son；M (g) is the quality of Cr-MOF/ wood composite aeroge；V (L) is the volume of testing liquid.
Fig. 4 is that Cr-MOF/ wood composite aeroge captures Pb2+Dynamic Adsorption curve.As seen from Figure 4, Cr-MOF/
Wood composite aeroge is to Pb2+Balance capture capacity increase sharply in a short time, be then slowly increased, finally realize most
Big balance capture ability.Cr-MOF/ wood composite aeroge is to Pb2+Maximum capture capacity be 3.64mmol/g.
Fig. 5 is that Cr-MOF/ wood composite aeroge captures Sr2+Dynamic Adsorption curve.Cr-MOF/ wood composite aeroge
To Sr2+Maximum capture capacity be 1.61mmol/g.
Fig. 6 is that Cr-MOF/ wood composite aeroge captures CS+Dynamic Adsorption curve.Cr-MOF/ wood composite aeroge
To CS+Maximum capture capacity be 0.41mmol/g.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme should all cover within the scope of the claims and the description of the invention.
Claims (10)
1. the preparation method that one kind can capture the Cr-MOF/ wood composite aeroge of heavy metal ion, which is characterized in that including such as
Lower step:
Step S1, desiccated wood is prepared into timber hydrogel；
Step S2, it is anti-that timber hydrogel immersion is contained to the solution that can form Cr-MOF progress hydro-thermal in sealing reactor
It answers, forms Cr-MOF/ wood composite hydrogel；
Step S3, the Cr-MOF/ wood composite hydrogel is dried, obtains Cr-MOF/ wood composite aeroge.
2. the preparation method of the Cr-MOF/ wood composite aeroge according to claim 1 for capturing heavy metal ion,
It is characterized in that, specific step is as follows by the step S1:
By the desiccated wood, successively acidified oxidant carries out acidification and lye carries out basification.
3. the preparation method of the Cr-MOF/ wood composite aeroge according to claim 1 for capturing heavy metal ion,
It is characterized in that, the moisture content of the desiccated wood in the step S1 is 0.1%~30%, and the type of the desiccated wood is poplar
Wood, birch, China fir or cork wood.
4. the preparation method of the Cr-MOF/ wood composite aeroge according to claim 2 for capturing heavy metal ion,
Be characterized in that, the acidification oxidant be hydrogen oxide, Peracetic acid, sodium dichromate, ammonium persulfate, sodium chlorite, sodium hypochlorite,
The pH of SODIUM PERCARBONATE, sodium perborate or potassium perborate, the acidification oxidant is 1.0~6.0, the quality of the acidification oxidant
Percentage is 0.1%~30%；
The temperature of the acidification is 20~100 DEG C, and the processing time is 1~120 hour.
5. the preparation method of the Cr-MOF/ wood composite aeroge according to claim 2 for capturing heavy metal ion,
It is characterized in that, the lye is lithium hydroxide, sodium hydroxide, potassium hydroxide or ammonium hydroxide, and the mass percent of the lye is 1%
~20%；
The temperature of the basification is 20~100 DEG C, and the processing time is 1~120 hour.
6. the preparation method of the Cr-MOF/ wood composite aeroge according to claim 1 for capturing heavy metal ion,
Be characterized in that, can be formed described in the step S2 Cr-MOF solution include molar ratio be 1:1:2 nine water chromic nitrates, 2- ammonia
Base terephthalic acid (TPA) and sodium hydroxide.
7. the preparation method of the Cr-MOF/ wood composite aeroge according to claim 1 for capturing heavy metal ion,
It is characterized in that, the temperature that hydro-thermal reaction is carried out in the step S2 is 50~200 DEG C, and the processing time is 1~120 hour.
8. the preparation method of the Cr-MOF/ wood composite aeroge according to claim 1 for capturing heavy metal ion,
It is characterized in that, the mode of the drying process in the step S3 is vacuum freeze drying, critical point drying or supercritical drying.
9. such as the system of the Cr-MOF/ wood composite aeroge of any of claims 1-8 for capturing heavy metal ion
Cr-MOF/ wood composite aeroge prepared by Preparation Method.
10. Cr-MOF/ wood composite aeroge as claimed in claim 9 is in the application for capturing heavy metal ion from sewage.
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| CN114210275A (en) * | 2021-10-21 | 2022-03-22 | 西南林业大学 | Method for preparing MOF/wood aerogel composite material |
| CN114259953A (en) * | 2021-12-31 | 2022-04-01 | 杭州电子科技大学 | P-CaCl2-Cr-MOF aerogel material, and preparation method and application thereof |
| CN114917887A (en) * | 2022-06-06 | 2022-08-19 | 南京林业大学 | Wood-based/MOF composite aerogel film and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114210275A (en) * | 2021-10-21 | 2022-03-22 | 西南林业大学 | Method for preparing MOF/wood aerogel composite material |
| CN114259953A (en) * | 2021-12-31 | 2022-04-01 | 杭州电子科技大学 | P-CaCl2-Cr-MOF aerogel material, and preparation method and application thereof |
| CN114917887A (en) * | 2022-06-06 | 2022-08-19 | 南京林业大学 | Wood-based/MOF composite aerogel film and preparation method thereof |
| CN114917887B (en) * | 2022-06-06 | 2023-08-18 | 南京林业大学 | Wood-based/MOF composite aerogel film and preparation method thereof |
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