CN107961765A - A kind of adsorbent and its green economy preparation method and application - Google Patents
A kind of adsorbent and its green economy preparation method and application Download PDFInfo
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- CN107961765A CN107961765A CN201711204650.8A CN201711204650A CN107961765A CN 107961765 A CN107961765 A CN 107961765A CN 201711204650 A CN201711204650 A CN 201711204650A CN 107961765 A CN107961765 A CN 107961765A
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- Prior art keywords
- adsorbent
- preparation
- ivy leaf
- boston ivy
- oxalic acid
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
-
- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0233—Compounds of Cu, Ag, Au
- B01J20/0237—Compounds of Cu
-
- 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
-
- 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
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
The invention discloses a kind of adsorbent and its green economy preparation method and application.The adsorbent is prepared according to the method included the following steps：Boston ivy leaf extract is obtained using water extraction Boston ivy leaf；Oxalic acid and and FeCl are added into the Boston ivy leaf extract3And CuCl2Mixed aqueous solution mix to obtain the final product.The present invention is using the Boston ivy leaf being generally easy to get as raw material, of low cost, easy to operate, non-toxic by-products；Meanwhile experiments verify that, the size of the adsorbent of preparation and oxalic acid are added with important relationship, and the addition of oxalic acid has a major impact the particle diameter for preparing sample particle.Adsorbent prepared by the present invention shows dyestuff higher absorption property, belongs to environmentally friendly material.Required equipment is simple in adsorbent preparation process of the present invention, easy to operate, and preparation speed is fast, and strong applicability is environmentally protective, is easy to be promoted the use of in actual life.
Description
Technical field
The present invention relates to a kind of adsorbent and its green economy preparation method and application, belong to Dye Adsorption technical field.
Background technology
Continuous with industrialization rhythm is accelerated, and the ecological environment around people is subject to serious destruction and pollution.According to
Report, the whole world is often close on hundreds of thousands ton waste water from dyestuff and is discharged into environment.And the dyestuff in waste water is to light and thermally stable, finally
Huge threat can be caused to ecological environment and human health, this severe situation promotes researcher to explore as early as possible can
The method for thoroughly and efficiently removing dyestuff.At present, the method for handling waste water from dyestuff is varied, including pre-oxidation, membrane filtration,
Absorption and coagulation-flocculation processing etc..But using toxic chemical or produce harmful by-products, energy consumption with the presence of many methods
And the defects of of high cost, wherein adsorption method is simple with its design, easily operated, it is efficient the advantages that, become processing dyestuff and give up
One of effective method of water.
In numerous adsorbents, nano material is due to its regular shape, surface area is big and the advantages that controlled porosity, into
One for high-efficiency adsorbent represents, and is subject to the extensive concern of researcher.So far, many nano materials include carbon nanometer
Pipe, graphene, metal oxide etc. are successfully prepared, and applied to the laboratory research of waste water from dyestuff reparation.However, these
The factors such as the complicated use with hazardous agents of the synthesis technique of method, seriously limit the large-scale production of these nano materials.
The adsorbent of economical and efficient, which is prepared, therefore, it is necessary to developing the feasible method of green meets the needs of environment remediation.
The content of the invention
Preparation of the Boston ivy leaf extract preparation using iron copper as the adsorbent of base is utilized the object of the present invention is to provide a kind of
Method, the present invention probe into it to the absorption malachite green dye performance for preparing sample by adding oxalic acid in the synthesis process
Influence.
Preparation method provided by the invention using iron copper as the adsorbent of base, includes the following steps：
Boston ivy leaf extract is obtained using water extraction Boston ivy leaf；Oxalic acid is added into the Boston ivy leaf extract
And and FeCl3And CuCl2Mixed aqueous solution mixing, that is, obtain the adsorbent using iron copper as base.
In above-mentioned preparation method, before the extraction, the Boston ivy leaf is through drying (to its mass conservation) and breaks
Broken processing.
In above-mentioned preparation method, in the extraction step, the dosage of the water is：Boston ivy leaf described in 1g needs 10
Water described in~40mL, if desired for water described in 17mL.
In above-mentioned preparation method, the condition of the extraction is as follows：
Temperature can be 50~80 DEG C；
When time can be 1~10 small, such as when extraction 2 is small under conditions of 80 DEG C.
In above-mentioned preparation method, the proportioning of the oxalic acid and the Boston ivy leaf extract is：Oxalic acid described in 1g：70~
Boston ivy leaf extract described in 650mL, such as 1g：635mL.
In above-mentioned preparation method, in the mixed aqueous solution, FeCl3Mass percentage be 1~5%, such as 2%,
CuCl2Mass percentage be 1~5%, such as 1.5%.
In above-mentioned preparation method, the volume ratio of the Boston ivy leaf extract and the mixed aqueous solution can be 1：0.05
~1, concretely 1：0.5~1 or 1：0.5.
In above-mentioned preparation method, 2~12h is stirred after the blend step, is dried after centrifugation.
The present invention is using the Boston ivy leaf being generally easy to get as raw material, of low cost, easy to operate, non-toxic by-products；Meanwhile
Experiments verify that the size and oxalic acid of the adsorbent of preparation are added with important relationship, the addition of oxalic acid is to preparing sample particle
Particle diameter have a major impact.
Adsorbent prepared by the present invention can effectively adsorb dyestuff, and especially malachite green dye is shown preferably to adsorb
Performance, can be used in the reparation of waste water from dyestuff.
The invention has the advantages that：
1st, the raw material used in preparation method of the present invention are easy to get, nontoxic, environmental protection, cheap, sharp again with waste recovery
The characteristics of using.
2nd, adsorbent prepared by the present invention shows dyestuff higher absorption property, belongs to environmentally friendly material.
3rd, required equipment is simple in adsorbent preparation process of the present invention, easy to operate, and preparation speed is fast, strong applicability, green
Environmental protection, is easy to be promoted the use of in actual life.
Brief description of the drawings
Fig. 1 is S prepared by the present invention1Sample (left figure) and S2The TEM figures of sample (right figure).
Fig. 2 is adsorption time in the embodiment of the present invention 2 to S1Sample and S2The influence of sample adsorption malachite green dye.
Fig. 3 is S in the embodiment of the present invention 22The dynamic analysis of sample adsorption MG dyestuffs.
Fig. 4 is S in the embodiment of the present invention 32Influence of the adsorbent input amount to the absorption property of dyestuff MG.
Fig. 5 is S in the embodiment of the present invention 42Adsorption capacity after sorbent circulation utilization.
Fig. 6 is S in the embodiment of the present invention 52The result of adsorbent stability.
Embodiment
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples, is commercially available unless otherwise specified.
Embodiment 1,
(1) preparation of Boston ivy leaf extract：Boston ivy leaf is gathered, the dust on surface is cleaned with distilled water, is dried to
Its mass conservation, then shreds, and weighs 12g dry leaves, is added in 200mL distilled water, is heated to 80 DEG C, when holding 2 is small,
Then filter, natural cooling, gained clarified solution is Boston ivy leaf extract.In addition, the oxalic acid for weighing 0.3152g is added to
In the Boston ivy leaf extract of 200mL, stirring is stand-by.
(2) green synthesis method is used to prepare the adsorbent using iron copper as base：By the Boston ivy leaf extract and grass of 200mL
The mixed liquor of acid is added dropwise to the FeCl of 100mL3(mass percentage 2%) and CuCl2(mass percentage is
1.5%) in mixed solution, it is uniformly mixed under agitation；12h, centrifugal filtration, by products therefrom are stirred under room temperature
Put into baking oven, 60 DEG C of dry 12h, grinding is stand-by, and gained sample is the adsorbent using iron copper as base, is denoted as S2Sample.
Repeat the above steps, Boston ivy leaf extract is directly added dropwise to FeCl by step in (2)3And CuCl2Mixed solution
In, obtained sample is denoted as S1Sample, as control sample.
As shown in Figure 1, left side and right side are respectively S1And S2The TEM figures of sample, understand, the sample topography of preparation through analysis
For particle；And S1Sample is compared, S2The grain diameter of sample is smaller, shows the addition of oxalic acid to preparing the grain of sample particle
Footpath has a major impact.
Embodiment 2,
Take 20mL 50mg/L MG (peacock green) solution to be placed in conical flask with cover, weigh the S of 6mg1Sample and S2Sample point
It Jia Ru not be placed in constant temperature oscillator, vibrated at a temperature of 30 DEG C in malachite green dye solution, one is taken out after a period of time
Divide solution, with the concentration of UV-VIS spectrophotometry test residual dye.Then, the operation is repeated, adsorption time is to absorption
Fig. 2 and Fig. 3 are shown in the influence result of capacity and its dynamic analysis.
As shown in Fig. 2, (1) is in increase trend with time growth in initial absorption phase, adsorption capacity.It is certain when reaching
Adsorption time after, adsorption capacity tends to balance.(2) in whole process, S2The adsorption capacity of sample was at initial one hour
Adsorption equilibrium is inside reached.The speed that the sample adsorption reaches balance is far longer than S1Sample.And S1Sample and S2Sample
Equilibrium adsorption capacities respectively may be about 110.15 and 166.57mg/g.Through dynamics model analysis, as shown in Figure 3, it is known that S2Sample
The process of absorption MG dyestuffs relatively meets first order kinetics curve.
Embodiment 3,
In a certain temperature conditions, influence of the adsorbent input amount to absorption dyestuff performance has been probed into.
First, at 30 DEG C, the S prepared is weighed2Sample 6mg, is added in 20mL50mg/L MG solution, is placed in and shakes
Swing and 12h is vibrated in device, precipitation and separation, the concentration for remaining malachite green dye is tested with UV-VIS spectrophotometry.Change sample
Addition between 0.05~0.7g/L, repeat above operation, experimental result is shown in Fig. 4.
As shown in Figure 4, the removal rate of MG increases with the increase of quantity of sorbent, this main and sample avtive spot
Increase related.On the contrary, the adsorption capacity of adsorbent is reduced as adsorbent addition increases, and this is primarily due to dyestuff point
Quantum count is certain, and as the quality increase of adsorbent, the adsorbent of unit mass can be obtained dye molecule reduction, and then
Show the reduction of adsorption capacity.
Embodiment 4,
Take the 50mg/L MG solution of certain volume to be placed in conical flask with cover, weigh the S of certain mass2Sample (0.3g/
L) add in malachite green dye solution, be placed in constant temperature oscillator, 12h is vibrated at a temperature of 30 DEG C, centrifuge, shift supernatant,
With the concentration of UV-VIS spectrophotometry test residual dye.For the precipitation of centrifugation gained, washed with absolute ethyl alcohol, directly
Become colorless to washing lotion color, then put the recycling sample (0.3g/L) for 60 DEG C of oven for drying, grinding, weighing certain mass,
The 50mg/L MG solution of certain volume is added to, repeats above step, circulation several times, records residual obtained by each loop test
The concentration of dyestuff.The result is shown in Fig. 5.
As shown in Figure 5, during loop test, S2To the absorption property of MG dyestuffs obvious become does not occur for sample
Change, adsorption capacity is always held near 162mg/g, it can be seen that, which has preferable reusing, this is in reality
It is very important in life.
Embodiment 5,
Take 20mL 50mg/L MG solution to be placed in conical flask with cover, weigh respectively the depositing in 1 in air of 6mg, 3,5,
7th, the S of 14,21,28 days2Sample (0.3g/L) is added in malachite green dye solution, is placed in constant temperature oscillator, in 30 DEG C of temperature
Lower vibration 12h, natural cooling, centrifugation, with the concentration of UV-VIS spectrophotometry test residual dye.The result is shown in Fig. 6.
As shown in fig. 6, the S of certain time is housed at room temperature2Sample all shows preferable adsorptivity to MG dyestuffs
Can, even if housing the nearly time of one month, obvious decline does not occur for sample adsorption performance.Illustrate the sample have compared with
Good stability.
Claims (10)
1. a kind of preparation method using iron copper as the adsorbent of base, includes the following steps：
Boston ivy leaf extract is obtained using water extraction Boston ivy leaf；Into the Boston ivy leaf extract add oxalic acid and with
FeCl3And CuCl2Mixed aqueous solution mixing, that is, obtain the adsorbent using iron copper as base.
2. preparation method according to claim 1, it is characterised in that：Before the extraction, the Boston ivy leaf is through dry
Dry and break process.
3. preparation method according to claim 1 or 2, it is characterised in that：In the extraction step, the dosage of the water
For：Boston ivy leaf described in 1g needs water described in 10~40mL.
4. preparation method according to any one of claim 1-3, it is characterised in that：The condition of the extraction is as follows：
Temperature is 50~80 DEG C；
When time is 1~10 small.
5. according to the preparation method any one of claim 1-4, it is characterised in that：The oxalic acid and the Boston ivy leaf
The proportioning of extracting solution is：Oxalic acid described in 1g：Boston ivy leaf extract described in 70~650mL.
6. according to the preparation method any one of claim 1-5, it is characterised in that：In the mixed aqueous solution, FeCl3
Mass percentage be 1~5%, CuCl2Mass percentage be 1~5%.
7. according to the preparation method any one of claim 1-6, it is characterised in that：The Boston ivy leaf extract and institute
The volume ratio for stating mixed aqueous solution is 1：0.05~1.
8. according to the preparation method any one of claim 1-7, it is characterised in that：After the blend step stirring 2~
12h, is dried after centrifugation.
9. adsorbent prepared by method any one of claim 1-8.
10. application of the adsorbent described in claim 9 in dye discoloration purification of waste water.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101810873A (en) * | 2010-03-09 | 2010-08-25 | 侯先槐 | Method for preparing natural plant deodorant |
| CN102202815A (en) * | 2008-05-16 | 2011-09-28 | 维鲁泰克技术股份有限公司 | Green synthesis of nanometals using plant extracts and use thereof |
| CN105126778A (en) * | 2015-07-13 | 2015-12-09 | 四川农业大学 | Preparation and application of several common plant extracts |
| CN105458283A (en) * | 2015-11-24 | 2016-04-06 | 太原理工大学 | Method for green synthesis of nanometer zero-valent iron-copper bi-metal material and application |
-
2017
- 2017-11-27 CN CN201711204650.8A patent/CN107961765A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102202815A (en) * | 2008-05-16 | 2011-09-28 | 维鲁泰克技术股份有限公司 | Green synthesis of nanometals using plant extracts and use thereof |
| CN101810873A (en) * | 2010-03-09 | 2010-08-25 | 侯先槐 | Method for preparing natural plant deodorant |
| CN105126778A (en) * | 2015-07-13 | 2015-12-09 | 四川农业大学 | Preparation and application of several common plant extracts |
| CN105458283A (en) * | 2015-11-24 | 2016-04-06 | 太原理工大学 | Method for green synthesis of nanometer zero-valent iron-copper bi-metal material and application |
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