CN105854822A - Method for preparing Cu<2+> adsorbent from corn stalk enzymolysis residue and application of Cu<2+> adsorbent - Google Patents
Method for preparing Cu<2+> adsorbent from corn stalk enzymolysis residue and application of Cu<2+> adsorbent Download PDFInfo
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- CN105854822A CN105854822A CN201610258060.2A CN201610258060A CN105854822A CN 105854822 A CN105854822 A CN 105854822A CN 201610258060 A CN201610258060 A CN 201610258060A CN 105854822 A CN105854822 A CN 105854822A
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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
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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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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Abstract
The invention discloses a method for preparing a Cu<2+> adsorbent from corn stalk enzymolysis residue and an application of the Cu<2+> adsorbent. The method comprises the steps: crushing the corn stalk enzymolysis residue, and carrying out screening, so as to obtain corn stalk enzymolysis residue powder; balancing moisture of the corn stalk enzymolysis residue powder, adding alkali liquor into the corn stalk enzymolysis residue powder, carrying out soaking, carrying out filtrating, adjusting the pH value of the filtrate to 1.5 so as to separate out precipitates, carrying out centrifugal separation, washing the precipitates with a hydrochloric solution, carrying out centrifugation, and carrying out freeze drying to remove moisture, so as to obtain enzymolysis lignin; then, adding the enzymolysis lignin, alkali liquor and epoxy chloropropane into a three-mouthed flask, carrying out a uniformly-stirred heating-up reaction, carrying out suction filtration, and then, carrying out clean washing, so as to obtain epoxy lignin; adding the epoxy lignin, alkali liquor and diethylenetriamine into a three-mouthed flask, carrying out a uniformly-stirred heating-up reaction, carrying out suction filtration, and then, carrying out clean washing, so as to obtain the adsorbent. The adsorbent has relatively high adsorption capacity to Cu<2+> in a solution and can be applied to the adsorptive separation and purification of Cu<2+> containing ionic wastewater.
Description
Technical field
The invention belongs to technical field of waste water processing, be specifically related to a kind of corn straw enzymolysis residue and prepare Cu2+Adsorbent
Method and application.
Background technology
Along with the most progressive of modern industry and development, the water become increasingly conspicuous pollutes to have become as and threatens people's orthobiosis
With the serious problems hindering socio-economic development.Various pollutant and toxicant in waste water are various, the most various organic
Dyestuff and heavy metal ion, bring certain threat to the life and health of the mankind, and this pollutant be at large natural environment
Lower very difficult by self degradation, prolongation over time brings no small harm necessarily to environment and human health.If to this
A little waste water are not acted upon, not only can polluted source, and can the health of the serious harm mankind.
At present, the mode processing the organic dyestuff in waste water and heavy metal ion mainly has membrane separation process, adds flocculant, electricity
The physics such as chemical method and biological treatment and chemical method.Traditional heavy metal waste water treatment process, such as Physical, chemical method
Deng generally having that cost is high, react secondary pollution slow, easy and the shortcoming such as low concentration wastewater is difficult.And enter by adding adsorbent
The absorption method of row adsorption treatment has energy and the advantage such as consumption of raw materials is low, operating cost is few, becomes the first-selection side that waste water processes
Method.Therefore finding renewable and degradable macromolecular material most important, living resources highlight as modified feedstock can not
The advantage substituted.
In recent years, timber and agricultural crop straw are carried out pretreatment, enzymolysis and fermenting and preparing biological ethanol to have carried out in a large number
Research, but remaining enzymolysis residue is many directly burns as fuel, the most low in economic efficiency, its effective ingredient is
To utilizing, and pollute environment.Along with stalk fermentation prepares the rapid rising of alcohol fuel industry, the high-valued profit of enzymolysis residue
With needing to cause the concern of people.This patent has carried out modification to enzymolysis residue, is prepared for that low cost, adsorption rate be fast, absorption
Measure big heavy metal absorbent.
Summary of the invention
The technical problem to be solved in the present invention be utilize corn straw enzymolysis residue prepare low cost, adsorption rate fast and
The Cu that adsorbance is big2+Adsorbent.This preparation method is simple and easy to operate, the easy circulation and stress of adsorbent of preparation, is adsorbed with organic dye
And heavy metal ion is rapidly and efficiently.The present invention also solves the technical problem that and there is provided this kind of adsorbent containing Cu2+Organic dyestuff
Application in processing with effluent containing heavy metal ions.
Technical scheme is as follows:
A kind of corn straw enzymolysis substrate prepares Cu2+The method of adsorbent, comprises the following steps:
S1. taking corn straw enzymolysis residue, mechanical activation comminution obtains corn straw enzymolysis residue powder, normal temperature drying environment bar
Store under part, standby；
S2. take S1 step gained corn straw enzymolysis residue powder, add aqueous slkali, constant temperature water bath soak extraction, filter,
Filtrate to 1.5-2.0 with hydrochloric acid solution regulation pH value, separates out precipitation, staticly settles at normal temperatures, the removal supernatant, centrifugal point
From, precipitation, first centrifugal with the hydrochloric acid solution washing of pH=2-3, then be centrifuged with distilled water wash, moisture removal is removed in lyophilization, i.e.
Obtain enzymolysis xylogen；
S3. adding enzymolysis xylogen, alkali liquor and epoxychloropropane in there-necked flask, uniform stirring heats up, reaction, sucking filtration
It is washed out totally obtaining epoxy lignin；
S4. adding epoxy lignin, alkali liquor and diethylenetriamine in there-necked flask, uniform stirring heats up, reaction, sucking filtration
It is washed out totally obtaining Cu2+Adsorbent.
In said method, described corn straw enzymolysis residue is the enzymolysis garbage that cellulosic ethanol preparation process produces.
In said method, the alkali liquor that S3 and S4 is used be mass fraction be the NaOH solution of 16.7%-20.0%.
In said method, the concentration of lye added in S2 step is 40-50g/mL-1, described corn straw enzymolysis residue powder
End and the solid-liquid ratio of alkali liquor are 1:40-1:50g/mL, and described bath temperature is 60-70 DEG C, and the described constant temperature soak extraction time is
2-3h。
In said method, enzymolysis xylogen in S3: alkali liquor: epoxychloropropane=1:10:10-1:15:15, described enzymolysis wood
The unit of quality is g, and the unit of described alkali liquor is mL, and the unit of described epoxychloropropane is mL, and described uniform stirring heats up and is
It is warming up to 80-85 DEG C of reaction 3-3.5h.
In said method, enzymolysis xylogen in S4: alkali liquor: diethylenetriamine=1:30:30-1:35:35, described enzymolysis wood
The unit of quality is g, and the unit of described alkali liquor is mL, and the unit of described diethylenetriamine is mL, and uniform stirring is warming up to 60-65
DEG C reaction 3-3.5h.
A kind of corn straw enzymolysis residue prepares Cu2+The Cu that the method for adsorbent prepares2+Adsorbent is applied to absorption
Cu in waste water2+。
In said method, analytical tool is laboratory disintegrator, Eppendorf AG 22331 type high speed centrifuge, constant temperature
Reaction oscillator, Germany's Zeiss company EVO18 type scanning electron microscope, Germany's Vector 33 type infrared spectrometer, Hitachi Z-2000
Flame/sampling Graphite Furnace Atomic Absorption spectrophotometer and other conventional analytical instruments.
The invention has the beneficial effects as follows:
Cu in Adsorbent For Removal of Heavy2+Absorption shows the outstanding advantages such as adsorption rate is fast, adsorption capacity is big, this prepares
Method is a kind of low cost, and raw material sources are extensive, mild condition, environmental friendliness.In a word, the present invention has mild condition, preparation
The advantages such as process is simple, strong innovation, practical.
Accompanying drawing explanation
Fig. 1 is corn straw enzymolysis residue and the Cu prepared2+The infrared spectrogram of adsorbent；
Fig. 2 is SEM figure (× 2000) of corn straw enzymolysis residue；
Fig. 3 is the Cu prepared2+Adsorbent SEM schemes (× 2000).
Detailed description of the invention
The present invention is further illustrated below in conjunction with the accompanying drawings with specific embodiment.Unless stated otherwise, the examination that the present invention uses
Agent and raw material are the conventional commercial reagent in this area and raw material.Unless stated otherwise, the percent related in the embodiment of the present invention
For mass percent.
Embodiment 1
Cu2+The preparation of adsorbent
Material choice: corn straw enzymolysis residue is the enzymolysis garbage produced in cellulosic ethanol preparation process.
1. the extraction of enzymolysis xylogen:
Weigh the raw material of 5.0g pretreatment, add the NaOH solution of 16.7%, solid-liquid ratio [corn straw enzymolysis residue powder
Quality (g): alkali liquor volume (mL)]=1:40, constant temperature soak extraction 2h at a temperature of 60 DEG C, to filter, filtrate is adjusted with hydrochloric acid solution
Joint pH value, to 1.5, separates out precipitation, stands overnight at normal temperatures, has substantially layering, removes the supernatant, centrifugation, and precipitation is first
Wash with the hydrochloric acid solution of pH=2 centrifugal, then be centrifuged with distilled water wash, be deposited in freeze drying box and be dried, i.e. obtain enzyme
Solve lignin.
2. the epoxidation reaction of enzymolysis xylogen:
Add in there-necked flask the enzymolysis xylogen of 5.0g, 50mL 16.7% alkali liquor and 50mL epoxychloropropane,
Uniform stirring is warming up to 80 DEG C of reaction 3.0h, sucking filtration, by 95% ethanol and distilled water wash extremely neutrality, checks with sodium thiosulfate
Remain without epoxychloropropane, cryodesiccated to epoxidation lignin by putting after product sucking filtration.
3. the aminating reaction of epoxidation lignin:
Weigh 1g epoxidation lignin, put in reactor, the alkali liquor of the 16.7% of addition 30mL and the diethyl of 30mL
Alkene triamine (DETA), uniform stirring is warming up to 60 DEG C of reaction 3.0h.After reaction terminates, use distilled water wash product, finally give
Adsorbent a.
Embodiment 2
Cu2+The preparation of adsorbent
Material choice: corn straw enzymolysis residue is the enzymolysis garbage produced in cellulosic ethanol preparation process.
1. the extraction of enzymolysis xylogen:
Weigh the raw material of 5.0g pretreatment, add the NaOH solution of 16.7%, solid-liquid ratio=1:50, perseverance at a temperature of 70 DEG C
Temperature soak extraction 2h, filters, and filtrate to 1.5 with hydrochloric acid solution regulation pH value, separates out precipitation, stands overnight at normal temperatures, have bright
Aobvious layering, removes the supernatant, centrifugation, and precipitation is first centrifugal with the hydrochloric acid solution washing of pH=2, then with distilled water wash from
The heart, is deposited in freeze drying box and is dried, i.e. obtain enzymolysis xylogen.
2. the epoxidation reaction of enzymolysis xylogen:
Add in there-necked flask the enzymolysis xylogen of 5.0g, 75mL 16.7% alkali liquor and 75mL epoxychloropropane,
Uniform stirring is warming up to 60 DEG C of reaction 3.0h, sucking filtration, by 95% ethanol and distilled water wash extremely neutrality, checks with sodium thiosulfate
Remain without epoxychloropropane, cryodesiccated to epoxidation lignin by putting after product sucking filtration.
3. the aminating reaction of epoxidation lignin:
Weigh 1g epoxidation lignin, put in reactor, the alkali liquor of the 16.7% of addition 40mL and the diethyl of 40mL
Alkene triamine (DETA), uniform stirring is warming up to 60 DEG C of reaction 3.0h.After reaction terminates, use distilled water wash product, finally give
Adsorbent b.
Embodiment 3
The adsorption reaction of adsorbent
First the tool plug ground conical flask of 4 cleaned 100mL, numbering 14 are taken.Being respectively configured concentration is 100mg/L
CuSO4Solution, adds CuSO the most respectively in each conical flask4The absorption obtained in solution and embodiment 1 and embodiment 2
Agent.
Concrete scheme is listed in table 1.
The reaction condition of table 1 absorption
By the condition of table 1, under conditions of the air baths of 30 DEG C and 400r/min, react in isothermal reaction oscillator
3h.After absorption terminates, filter out the black solid in solution, obtain the solution of clear.Use the Z-of HIT
2000 type flame atomic absorption spectrometries, survey Cu in solution2+Concentration, test result is shown in Table 2.
Cu after table 2 absorption2+Concentration
Adsorption capacity=V* (C0-C1)/W
In formula: the volume of V metal ion solution, L； C0Cu in solution2+Mass concentration mg/L
C1Cu after absorption2+Mass concentration mg/L W sample quality, g
As can be seen from the table, after adding adsorbent, Cu in solution2+Concentration substantially reduces, and illustrates that adsorbent is to Cu2+
Having the strongest absorbability, adsorption capacity is up to 40-47.5mg/g, and the adsorbent of synthesis is a kind of good Cu2+Adsorbent.
Embodiment 4
The adsorption reaction of adsorbent
Power taking waste electroplating 50mL, in conical flask, is subsequently adding 50mg adsorbent, rotates adsorption reaction 3h, survey at 30 DEG C
Cu in waste water before and after fixed absorption2+Content.
Cu before and after table 2 absorption2+Concentration
As can be seen from the table, after electroplating wastewater adds adsorbent agent, Cu in solution2+Concentration substantially reduces, and says
Bright adsorbent is to Cu2+Having certain absorbability, adsorption capacity is up to 49.1mg/g, and the adsorbent of synthesis is a kind of good
Cu2+Adsorbent.
Embodiment 5
The FTIR spectrum detection of adsorbent and scanning electron microscope detect
The adsorbent a obtained in Example 1, uses Vector 33 type infrared spectrometer (Bruker company of Germany) right
Sample carries out infrared analysis.Scanning wavelength scope: 4000-400cm-1, resolution 0.3cm-1, signal to noise ratio 30000: 1, use bromine
Change potassium pressed disc method and prepare sample, amount of samples 1.5mg/350mg KBr.
The adsorbent a obtained in Example 1, first carries out powder sample surface gold-plating, then uses EVO18 type scanning electricity
Sample is analyzed by scarnning mirror ultramicroscope (Zeiss company of Germany).Accelerating potential is 10kV, and resolution is 3nm.
From the FTIR spectrum analysis of Fig. 1 it can be seen that according to document, by the infrared spectrum feature of enzymolysis residue and adsorbent
Absworption peak is summarized in table 3.
At 797cm-1、1127cm-1、1654cm-1And 3400cm-1The absworption peak at place is remarkably reinforced, and these are all the spies of amido
Levying absworption peak, illustrate under the catalysis of alkali, the epoxy radicals of epoxidation lignin is attacked and open loop, enzymolysis by the amine that nucleophilicity is the strongest
The aminated compounds that residue is formed.The appearance of these characteristic peaks may certify that diethylenetriamine has grafted on lignin.
From the point of view of the scanning electron microscopic picture of Fig. 2 and Fig. 3, unmodified enzymolysis residue presents the graininess of gathering, structure
Dense.There are cellular and some gap structures in modified adsorbent, and this is owing to, in modifying process, lignin there occurs
Cross-linking reaction, meanwhile, amination modifying makes the surface of lignin ratio more loose amido, carboxyl occur so that it is have certain hydrophilic
Property, cause the change of material surface form.So there is the more loose vesicular texture of ratio, this structure in modified adsorbent
The surface area making lignin increases, and is more beneficial for contacting with solution, improves the Cu in waste water2+Adsorbance.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by above-described embodiment
Limit, the change made under other any spirit without departing from the present invention and principle, modify, substitute, combine, simplify,
All should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (7)
1. a corn straw enzymolysis substrate prepares Cu2+The method of adsorbent, it is characterised in that comprise the following steps:
S1. taking corn straw enzymolysis residue, mechanical activation comminution obtains corn straw enzymolysis residue powder, normal temperature drying environmental condition
Lower storage, standby；
S2. take S1 step gained corn straw enzymolysis residue powder, add aqueous slkali, constant temperature water bath soak extraction, filter, filtrate
By hydrochloric acid solution regulation pH value to 1.5-2.0, separate out precipitation, staticly settle at normal temperatures, the removal supernatant, centrifugal point
From, precipitation, first centrifugal with the hydrochloric acid solution washing of pH=2-3, then be centrifuged with distilled water wash, moisture removal is removed in lyophilization, i.e.
Obtain enzymolysis xylogen；
S3. adding enzymolysis xylogen, alkali liquor and epoxychloropropane in there-necked flask, uniform stirring heats up, and reaction, sucking filtration is then
Washes clean obtains epoxy lignin；
S4. adding epoxy lignin, alkali liquor and diethylenetriamine in there-necked flask, uniform stirring heats up, and reaction, sucking filtration is right
Rear washes clean obtains Cu2+Adsorbent.
The most according to claim 1, a kind of corn straw enzymolysis residue prepares Cu2+The method of adsorbent, it is characterised in that institute
Stating corn straw enzymolysis residue is the enzymolysis garbage that cellulosic ethanol preparation process produces.
The most according to claim 1, a kind of corn straw enzymolysis residue prepares Cu2+The method of adsorbent, it is characterised in that S3
The alkali liquor used with S4 be mass fraction be the NaOH solution of 16.7%-20.0%.
The most according to claim 1, a kind of corn straw enzymolysis residue prepares Cu2+The method of adsorbent, it is characterised in that S2
The concentration of lye added in step is 40-50g/mL-1, described corn straw enzymolysis residue powder is 1 with the solid-liquid ratio of alkali liquor:
40-1:50g/mL, described bath temperature is 60-70 DEG C, and the described constant temperature soak extraction time is 2-3h.
The most according to claim 1, a kind of corn straw enzymolysis residue prepares Cu2+The method of adsorbent, it is characterised in that S3
Middle enzymolysis xylogen: alkali liquor: epoxychloropropane=1:10:10-1:15:15, the unit of described enzymolysis xylogen is g, described alkali liquor
Unit be mL, the unit of described epoxychloropropane is mL, described uniform stirring heat up for be warming up to 80-85 DEG C react 3-
3.5h。
The most according to claim 1, a kind of corn straw enzymolysis residue prepares Cu2+The method of adsorbent, it is characterised in that S4
Middle enzymolysis xylogen: alkali liquor: diethylenetriamine=1:30:30-1:35:35, the unit of described enzymolysis xylogen is g, described alkali liquor
Unit be mL, the unit of described diethylenetriamine is mL, uniform stirring be warming up to 60-65 DEG C reaction 3-3.5h.
7. described in claim 1, a kind of corn straw enzymolysis residue prepares Cu2+The Cu that the method for adsorbent prepares2+Adsorbent
It is applied to adsorb Cu in waste water2+。
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106883376A (en) * | 2017-02-21 | 2017-06-23 | 江苏迪因生物科技有限公司 | The preparation method of enzymolysis xylogen base epoxy |
| CN108503395A (en) * | 2018-05-16 | 2018-09-07 | 芜湖市创源新材料有限公司 | A method of to digest residue oxidation product polypeptide-amino acids metal ion chelating liquid fertilizer is prepared as chelating agent |
| CN109485065A (en) * | 2017-09-09 | 2019-03-19 | 中国石油化工股份有限公司 | A kind of multistage porous molecular sieve and preparation method thereof |
| CN110170303A (en) * | 2019-06-10 | 2019-08-27 | 陕西科技大学 | A kind of heavy-metal adsorption material and its preparation method and application |
| CN110773133A (en) * | 2019-11-27 | 2020-02-11 | 深圳信息职业技术学院 | Preparation method of dye wastewater adsorbent and purification method of dye wastewater |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106883376A (en) * | 2017-02-21 | 2017-06-23 | 江苏迪因生物科技有限公司 | The preparation method of enzymolysis xylogen base epoxy |
| CN106883376B (en) * | 2017-02-21 | 2019-01-25 | 山西舜质新材料科技有限公司 | The preparation method of enzymolysis xylogen base epoxy |
| CN109485065A (en) * | 2017-09-09 | 2019-03-19 | 中国石油化工股份有限公司 | A kind of multistage porous molecular sieve and preparation method thereof |
| CN109485065B (en) * | 2017-09-09 | 2021-03-05 | 中国石油化工股份有限公司 | Hierarchical pore molecular sieve and preparation method thereof |
| CN108503395A (en) * | 2018-05-16 | 2018-09-07 | 芜湖市创源新材料有限公司 | A method of to digest residue oxidation product polypeptide-amino acids metal ion chelating liquid fertilizer is prepared as chelating agent |
| CN110170303A (en) * | 2019-06-10 | 2019-08-27 | 陕西科技大学 | A kind of heavy-metal adsorption material and its preparation method and application |
| CN110773133A (en) * | 2019-11-27 | 2020-02-11 | 深圳信息职业技术学院 | Preparation method of dye wastewater adsorbent and purification method of dye wastewater |
| CN110773133B (en) * | 2019-11-27 | 2022-09-30 | 深圳信息职业技术学院 | Preparation method of dye wastewater adsorbent and purification method of dye wastewater |
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Application publication date: 20160817 |
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