CN104667898B - A kind of preparation method of eucalyptus base porous carbon-Silica solid phase extraction column - Google Patents
A kind of preparation method of eucalyptus base porous carbon-Silica solid phase extraction column Download PDFInfo
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- CN104667898B CN104667898B CN201510060603.5A CN201510060603A CN104667898B CN 104667898 B CN104667898 B CN 104667898B CN 201510060603 A CN201510060603 A CN 201510060603A CN 104667898 B CN104667898 B CN 104667898B
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- eucalyptus
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Abstract
The invention discloses a kind of preparation methods of eucalyptus base porous carbon-Silica solid phase extraction column.Method is as follows: 1) it into eucalyptus bar is added zinc chloride, is activated under conditions of hydro-thermal, washed, it is dry, and it pulverizes;Sodium hydroxide is added, mixes well, is made into column;It is put into atmosphere furnace, nitrogen protection, at high temperature calcination;Natural cooling is taken out, washes away sodium hydroxide with hydrochloric acid, dries, and obtains eucalyptus base porous carbon;2) nitration mixture is added into porous carbon, it is activated, washes away extra nitration mixture, it is dry, for use;3) porous carbon is mixed into mixing with silica, be attached in polyethylene solid phase extraction tube, in addition eucalyptus base porous carbon-Silica solid phase extraction column is made in sieve plate, compacting.The advantages that low cost product is easy to get, is easy to operate, process flow is simple, favorable reproducibility and pollution are small, has very strong practicability.
Description
Technical field
The present invention relates to the preparation technical field of solid-phase extraction column more particularly to a kind of eucalyptus base porous carbon-silica
The preparation method of solid-phase extraction column.
Background technique
Most of the filler of solid-phase extraction column used at present is: silica filler, polymer filler, aluminium oxide, active carbon,
Diatomite etc..But mostly there is preparation complexity, disadvantages at high cost.
With the reduction of the mineral resources such as petroleum, coal, the utilization of biomass resource is increasingly taken seriously.In state's housekeeping
Under the guidance of plan, my area's most recent two decades plant eucalyptus energetically, and growth is fast, resourceful.It is a kind of economic function woods, according to not
Statistics, whole district's eucalyptus area in 2011 have reached to more than 180 ten thousand hm completely2, account for the 1/4 of the artificial Commercial Forests area of the whole district, eucalyptus
Timber yield accounts for the 2/3 of whole district's timber yield, and area and yield all rank first in the country.Eucalyptus is presently mainly to be processed with timber
Based on, prefabricated board, building slab, papermaking and paper pulp etc..After transporting a large amount of trunk, a large amount of branches and leaves, branch, saw are left
How do the residues such as end, bark handle these residues? resource utilization is improved, the income of self-employed tree cultivator and enterprise are increased.Therefore,
If converting porous carbon for them, a kind of efficient small-sized solid-phase extraction column is developed, these resources will be more fully utilized,
Bigger income is brought to agriculture and forestry.
Summary of the invention
The present invention provides a kind of preparation methods of eucalyptus base porous carbon-Silica solid phase extraction column.The present invention is with big
The cheap eucalyptus waste of amount is raw material, prepares eucalyptus base porous carbon-Silica solid phase using simple reaction process
Extraction column has good adsorption effect not only for heavy metal ion, also has all well and good effect for industrial wastewater dyestuff
Fruit.
The present invention adopts the following technical scheme:
Specific step is as follows for eucalyptus base porous carbon-Silica solid phase extraction column preparation method of the invention:
(1) preparation of eucalyptus base porous carbon:
Using eucalyptus bar as raw material, zinc chloride is added and changes in advance, is activated 1-3 hours under conditions of hydro-thermal, washs, it is dry, it grinds
It is broken, obtain preactivated eucalyptus bar powder;Sodium hydroxide is added into preactivated eucalyptus bar powder, mixes well, is made into column
Shape;Eucalyptus powder column is put into atmosphere furnace, nitrogen protection, at high temperature calcination;Natural cooling is taken out, with salt pickling
Sodium hydroxide is removed, is dried, eucalyptus base porous carbon is obtained;
(2) activation of eucalyptus base porous carbon:
Nitration mixture is added into the eucalyptus base porous carbon of step (1) preparation, it is activated, eucalyptus Quito hole carbon surface is made
Increase carboxyl, hydroxyl group, improves adsorbance;Extra nitration mixture is washed away, it is dry, for use;
(3) eucalyptus base porous carbon-Silica solid phase extraction column preparation:
Eucalyptus base porous carbon after step (2) activation is mixed into mixing with silica, is attached to polyethylene solid phase extraction tube
In, in addition eucalyptus base porous carbon-Silica solid phase extraction column is made in sieve plate, compacting.
In step (1), the weight ratio of eucalyptus bar and zinc chloride is 0.5~2:1;The temperature of hydro-thermal is 100~200 degree;It grinds
Partial size after broken is 5mm;It with the weight ratio of sodium hydroxide is 0.5~2:1 in preactivated eucalyptus bar powder;The temperature of high temperature sintering
Degree and time are 600-1100 degree, 2h respectively.
In step (2), the nitration mixture is made of sulfuric acid, nitric acid, the w/v of eucalyptus base porous carbon and nitration mixture
It is 0.5-2:1mg/ml;Activation time is 4-8h.
In step (3), the silica the preparation method is as follows: every addition 10-20ml ethyl alcohol in the reactor, right
100-1000ul water should be added, 100-1000ul ammonium hydroxide is added 200-700ul TEOS after mixing evenly, reacts at room temperature 5-
12h is centrifuged 5 minutes after reaction, takes lower sediment, ultrasonic disperse in ethanol, then is centrifuged, and 4 times repeatedly, lower layer is sunk
Shallow lake N2Drying, obtains silica.
In step (3), the ratio of eucalyptus base porous carbon and silica after activation is: after every 0.005-0.2g activation
Eucalyptus base porous carbon corresponds to 0.005-0.2g silica.
The present invention by porous carbon with silica is full and uniform be blended after filling be successfully prepared eucalyptus base porous carbon-dioxy
The raw material for preparing of SiClx solid-phase extraction column, the solid-phase extraction column is easy to get, and eucalyptus base porous carbon is adequately mixed with silica
It closes, mutually supports, there is certain gap, the super large surface area based on porous carbon has the adsorption capacity of super large.
The positive effect of the present invention is as follows:
Compared with traditional filler, have the advantage that
(1) raw material sources for preparing porous carbon are wide, it is cheap be easy to get, simple process, it is pollution-free.
(2) method of silica is simple, mature.
(3) solid-phase extraction column prepared by is at low cost, large amount of adsorption.
(4) preparation process is fairly simple, easy to operate, favorable reproducibility and pollutes small, cheaper.Suitable market pushes away
Extensively, the masses of the people is benefited from.
(5) eucalyptus base porous carbon-Silica solid phase extraction column preparation process of the invention is simple, and raw material sources are wide
General, required laboratory apparatus is also fairly simple, can be used for being mass produced.
(6) absorption object is combined closely by complexing and physisorption power porous carbon, is advantageously implemented absorption
Object good absorption is eluted using organic solvent or diluted acid, detection.
(7) eucalyptus base porous carbon-Silica solid phase extraction column that this method is prepared, makes full use of local characteristic to provide
Traditional waste is become useful product, improves the added value of agricultural product by source.
Detailed description of the invention
Fig. 1 is the Raman spectrogram of the eucalyptus base porous carbon prepared under different temperatures.
Fig. 2 is the XRD spectra of the eucalyptus base porous carbon prepared under different temperatures.
Specific embodiment
The following examples are a further detailed description of the invention.
Embodiment 1
Specific step is as follows for eucalyptus base porous carbon-Silica solid phase extraction column preparation method of the invention:
(1) preparation of eucalyptus base porous carbon:
Using eucalyptus bar as raw material, zinc chloride is added and changes in advance, is activated 1 hour under conditions of hydro-thermal, washs, it is dry, it pulverizes,
Obtain preactivated eucalyptus bar powder;Sodium hydroxide is added into preactivated eucalyptus bar powder, mixes well, is made into column;
Eucalyptus powder column is put into atmosphere furnace, nitrogen protection, at high temperature calcination;Natural cooling is taken out, washes away hydrogen with hydrochloric acid
Sodium oxide molybdena, drying obtain eucalyptus base porous carbon;
(2) activation of eucalyptus base porous carbon:
Nitration mixture is added into the eucalyptus base porous carbon of step (1) preparation, it is activated, eucalyptus base porous carbon table is made
Face increases carboxyl, hydroxyl group, improves adsorbance;Extra nitration mixture is washed away, it is dry, for use;
(3) eucalyptus base porous carbon-Silica solid phase extraction column preparation:
Eucalyptus base porous carbon after step (2) activation is mixed into mixing with silica, is attached to polyethylene solid phase extraction tube
In, in addition eucalyptus base porous carbon-Silica solid phase extraction column is made in sieve plate, compacting.
In step (1), the weight ratio of eucalyptus bar and zinc chloride is 0.5:1;The temperature of hydro-thermal is 100 degree;Grain after pulverizing
Diameter is 5mm;It with the weight ratio of sodium hydroxide is 0.5:1 in preactivated eucalyptus bar powder;The temperature and time of high temperature sintering point
It is not 600 degree, 2h.
In step (2), the nitration mixture is made of sulfuric acid, nitric acid, the w/v of eucalyptus base porous carbon and nitration mixture
It is 0.5:1mg/ml;Activation time is 4h.
In step (3), the silica the preparation method is as follows: every addition 10ml ethyl alcohol in the reactor, corresponding
100ul water is added, 100ul ammonium hydroxide is added 200ul TEOS after mixing evenly, reacts at room temperature 5h, after reaction, is centrifuged 5 points
Clock takes lower sediment, and ultrasonic disperse in ethanol, then is centrifuged, and 4 times repeatedly, by lower sediment N2Drying, obtains titanium dioxide
Silicon.
In step (3), the ratio of eucalyptus base porous carbon and silica after activation is: the eucalyptus after every 0.005g activation
Base porous carbon corresponds to 0.005g silica.
Embodiment 2
Specific step is as follows for eucalyptus base porous carbon-Silica solid phase extraction column preparation method of the invention:
(1) preparation of eucalyptus base porous carbon:
Using eucalyptus bar as raw material, zinc chloride is added and changes in advance, is activated 3 hours under conditions of hydro-thermal, washs, it is dry, it pulverizes,
Obtain preactivated eucalyptus bar powder;Sodium hydroxide is added into preactivated eucalyptus bar powder, mixes well, is made into column;
Eucalyptus powder column is put into atmosphere furnace, nitrogen protection, at high temperature calcination;Natural cooling is taken out, washes away hydrogen with hydrochloric acid
Sodium oxide molybdena, drying obtain eucalyptus base porous carbon;
(2) activation of eucalyptus base porous carbon:
Nitration mixture is added into the eucalyptus base porous carbon of step (1) preparation, it is activated, eucalyptus Quito hole carbon surface is made
Increase carboxyl, hydroxyl group, improves adsorbance;Extra nitration mixture is washed away, it is dry, for use;
(3) eucalyptus base porous carbon-Silica solid phase extraction column preparation:
Eucalyptus base porous carbon after step (2) activation is mixed into mixing with silica, is attached to polyethylene solid phase extraction tube
In, in addition eucalyptus base porous carbon-Silica solid phase extraction column is made in sieve plate, compacting.
In step (1), the weight ratio of eucalyptus bar and zinc chloride is 2:1;The temperature of hydro-thermal is 200 degree;Partial size after pulverizing
It is 5mm;It with the weight ratio of sodium hydroxide is 2:1 in preactivated eucalyptus bar powder;The temperature and time of high temperature sintering is respectively
1100 degree, 2h.
In step (2), the nitration mixture is made of sulfuric acid, nitric acid, the w/v of eucalyptus base porous carbon and nitration mixture
2:1mg/ml;Activation time is 8h.
In step (3), the silica the preparation method is as follows: every addition 20ml ethyl alcohol in the reactor, corresponding
1000ul water is added, 1000ul ammonium hydroxide is added 700ul TEOS after mixing evenly, reacts at room temperature 12h, after reaction, centrifugation
5 minutes, lower sediment is taken, ultrasonic disperse in ethanol, then is centrifuged, and 4 times repeatedly, by lower sediment N2Drying, obtains dioxy
SiClx.
In step (3), the ratio of eucalyptus base porous carbon and silica after activation is: the eucalyptus base after every 0.2g activation
Porous carbon corresponds to 0.005g silica.
Embodiment 3
Specific step is as follows for eucalyptus base porous carbon-Silica solid phase extraction column preparation method of the invention:
(1) preparation of eucalyptus base porous carbon:
Using eucalyptus bar as raw material, zinc chloride is added and changes in advance, is activated 2 hours under conditions of hydro-thermal, washs, it is dry, it pulverizes,
Obtain preactivated eucalyptus bar powder;Sodium hydroxide is added into preactivated eucalyptus bar powder, mixes well, is made into column;
Eucalyptus powder column is put into atmosphere furnace, nitrogen protection, at high temperature calcination;Natural cooling is taken out, washes away hydrogen with hydrochloric acid
Sodium oxide molybdena, drying obtain eucalyptus base porous carbon;
(2) activation of eucalyptus base porous carbon:
Nitration mixture is added into the eucalyptus base porous carbon of step (1) preparation, it is activated, eucalyptus Quito hole carbon surface is made
Increase carboxyl, hydroxyl group, improves adsorbance;Extra nitration mixture is washed away, it is dry, for use;
(3) eucalyptus base porous carbon-Silica solid phase extraction column preparation:
Eucalyptus base porous carbon after step (2) activation is mixed into mixing with silica, is attached to polyethylene solid phase extraction tube
In, in addition eucalyptus base porous carbon-Silica solid phase extraction column is made in sieve plate, compacting.
In step (1), the weight ratio of eucalyptus bar and zinc chloride is 1:1;The temperature of hydro-thermal is 150 degree;Partial size after pulverizing
It is 5mm;It with the weight ratio of sodium hydroxide is 1:1 in preactivated eucalyptus bar powder;The temperature and time of high temperature sintering is respectively
900 degree, 2h.
In step (2), the nitration mixture is made of sulfuric acid, nitric acid, the w/v of eucalyptus base porous carbon and nitration mixture
1:1mg/ml;Activation time is 6h.
In step (3), the silica the preparation method is as follows: every addition 15ml ethyl alcohol in the reactor, corresponding
500ul water is added, 500ul ammonium hydroxide is added 400ul TEOS after mixing evenly, reacts at room temperature 9h, after reaction, is centrifuged 5 points
Clock takes lower sediment, and ultrasonic disperse in ethanol, then is centrifuged, and 4 times repeatedly, by lower sediment N2Drying, obtains titanium dioxide
Silicon.
In step (3), the ratio of eucalyptus base porous carbon and silica after activation is: the eucalyptus after every 0.005g activation
Base porous carbon corresponds to 0.2g silica.
Using Raman spectrometer to the characterization of porous carbon in experiment, as shown in Figure 1, as the temperature rises, the ratio of ID/IG
It is worth smaller and smaller, peak degree of separation is higher and higher, it was demonstrated that its degree of graphitization is higher and higher to obtain graphited porous carbon.
As shown in Fig. 2, X diffraction curve has 2 diffraction maximums at 24 ° and 44 °, correspond respectively to graphite (002),
(101) crystal face, their intensity increase as the temperature rises and significantly, meanwhile, 002 crystal face is as temperature is gradually to 26.5 °
Offset, further proves graphited raising.
Porous carbon synthesized by the present invention passes through specific surface instrument measurement the specific area, the results showed that, specific surface area is in 1200-
2000m2/ g illustrates bigger specific surface area.
Selecting lead ion is the object for assessing solid-phase extraction column, from the capacity of pillar, adsorption flow rate, elution flow rate, repetition
Property etc. conditions investigate, the results showed that the product show adsorption capacity larger (80-200mg/L), favorable reproducibility (3-5 times) and
The advantages that small is polluted, there is very strong practicability, improve the added value of agricultural product.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (5)
1. a kind of preparation method of eucalyptus base porous carbon-Silica solid phase extraction column, it is characterised in that: the method it is specific
Steps are as follows:
(1) preparation of eucalyptus base porous carbon:
Using eucalyptus bar as raw material, zinc chloride is added and changes in advance, is activated 1-3 hours under conditions of hydro-thermal, washs, it is dry, it pulverizes, obtains
To preactivated eucalyptus bar powder;Sodium hydroxide is added into preactivated eucalyptus bar powder, mixes well, is made into column;It will
Eucalyptus powder column is put into atmosphere furnace, nitrogen protection, at high temperature calcination;Natural cooling is taken out, washes away hydrogen-oxygen with hydrochloric acid
Change sodium, drying obtains eucalyptus base porous carbon;
(2) activation of eucalyptus base porous carbon:
Nitration mixture is added into the eucalyptus base porous carbon of step (1) preparation, it is activated, increases eucalyptus Quito hole carbon surface
Carboxyl, hydroxyl group improve adsorbance;Extra nitration mixture is washed away, it is dry, for use;
(3) eucalyptus base porous carbon-Silica solid phase extraction column preparation:
Eucalyptus base porous carbon after step (2) activation is mixed into mixing with silica, is attached in polyethylene solid phase extraction tube, adds
Eucalyptus base porous carbon-Silica solid phase extraction column is made in upper sieve plate, compacting.
2. the preparation method of eucalyptus base porous carbon-Silica solid phase extraction column as described in claim 1, it is characterised in that:
In step (1), the weight ratio of eucalyptus bar and zinc chloride is 0.5~2:1;The temperature of hydro-thermal is 100~200 DEG C;After pulverizing
Partial size be 5mm;It with the weight ratio of sodium hydroxide is 0.5~2:1 in preactivated eucalyptus bar powder;The temperature of high temperature sintering and
Time is 600-1100 DEG C respectively, 2h.
3. the preparation method of eucalyptus base porous carbon-Silica solid phase extraction column as described in claim 1, it is characterised in that:
In step (2), the nitration mixture is made of sulfuric acid, nitric acid, and the w/v of eucalyptus base porous carbon and nitration mixture is 0.5-2:
1mg/mL ;Activation time is 4-8h.
4. the preparation method of eucalyptus base porous carbon-Silica solid phase extraction column as described in claim 1, it is characterised in that:
In step (3), the silica the preparation method is as follows: every addition 10-20mL ethyl alcohol in the reactor, corresponding to be added
100-1000 μ L water, 100-1000 μ L ammonium hydroxide are added 200-700 μ L TEOS after mixing evenly, react at room temperature 5-12h, instead
After answering, it is centrifuged 5 minutes, takes lower sediment, ultrasonic disperse in ethanol, then is centrifuged, and 4 times repeatedly, by lower sediment N2
Drying, obtains silica.
5. the preparation method of eucalyptus base porous carbon-Silica solid phase extraction column as described in claim 1, it is characterised in that:
In step (3), the ratio of eucalyptus base porous carbon and silica after activation is: eucalyptus Quito after every 0.005-0.2g activation
Hole carbon corresponds to 0.005-0.2g silica.
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