CN110170315A - A kind of fiber base aeroge adsorbent and its application in absorption dyeing waste-water - Google Patents
A kind of fiber base aeroge adsorbent and its application in absorption dyeing waste-water Download PDFInfo
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- CN110170315A CN110170315A CN201910300252.9A CN201910300252A CN110170315A CN 110170315 A CN110170315 A CN 110170315A CN 201910300252 A CN201910300252 A CN 201910300252A CN 110170315 A CN110170315 A CN 110170315A
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
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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
- B01J20/28—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
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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
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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
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- 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
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
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Abstract
The present invention relates to field of material technology, disclose a kind of fiber base aeroge adsorbent and its application in absorption dyeing waste-water.Fiber base aeroge adsorbent of the invention is prepared by cellulose, acrylic acid and acrylamide by polymerization reaction, and wherein the mass ratio of cellulose, acrylic acid and acrylamide is 1:8 ~ 12:1 ~ 3.It is 900 ~ 1100mg L by fiber base aeroge adsorbent investment concentration‑1Methylene blue solution in, in 60min, 775 ~ 786g/g is reached to the adsorbance of methylene blue.The present invention passes through MOLECULE DESIGN, functional functional group is introduced in cellulosic molecule, pass through technology controlling and process, the cellulose base adsorbent material of high efficiency of additive capability is obtained, realizes the dual purpose for the treatment of wastes with processes of wastes against one another that the recycling and reuse to containing cellulose weaving waste resource are combined to the efficient quick removal to dyes in dyeing waste water.
Description
Technical field
It gives up the present invention relates to field of material technology more particularly to a kind of fiber base aeroge adsorbent and its in absorption dyeing
Application in water.
Background technique
Aerogel material is the three-dimensional network knot for replacing the liquid inside gel to collapse without hole gas
Structure material has the characteristics that specific surface area is high, density is small, thermal conductivity is low and dielectric constant is low.Inorganic aerogels density is relatively
Greatly, structure is more crisp, and organic polymer Mechanical Properties of Aerogels is relatively weak, non-refractory.Cellulose aerogels are made with cellulose
It is low in cost for raw material, it is from a wealth of sources, there is excellent biological sexual clorminance and good mechanical strength, toughness is more preferable, a variety of
Advantage is had more in industry application.
Chinese invention patent application number is the patent of CN201410227554.5, discloses a kind of alginate fibre element aeroge
The preparation method of oil absorption material, preparation method includes the following steps: the purifying of alginate fibre element；Machinery glue mill preparation seaweed receives
Rice cellulose microfibril；The preparation of alginate fibre element aeroge；The hydrophobically modified of alginate fibre element aeroge.Alginate fibre element
Aeroge oil absorption material have many advantages, such as oil absorption efficiency it is high, it is natural it is pollution-free, intensity is good, secondary treatment is simple.However, this method
It cannot achieve the recycling and reuse to containing cellulose weaving waste resource.
Summary of the invention
It is dyed in order to solve the above-mentioned technical problems, the present invention provides a kind of fiber base aeroge adsorbent and its in absorption
Application in waste water.The present invention introduces functional functional group and in fiber base airsetting by MOLECULE DESIGN in cellulosic molecule
Modified activated carbon is introduced in glue adsorbent, by technology controlling and process, obtains the cellulose that there is high efficiency of additive capability to dyeing waste-water
Adsorbing material.
The specific technical proposal of the invention is: a kind of fiber base aeroge adsorbent, the fiber base aeroge adsorbent
It is prepared by cellulose, acrylic acid and acrylamide by polymerization reaction, wherein the matter of cellulose, acrylic acid and acrylamide
Amount is than being 1: 8~12: 1~3.
The present invention is raw material using waste cellulose, by grafted propylene acid and acrylamide, prepares cellulose base absorption
Agent, the removal for dope dyeing Wastewater Dyes.By MOLECULE DESIGN, functional functional group is introduced in cellulosic molecule
(amino, carboxyl, hydroxyl) obtains the cellulose base adsorbent material of high efficiency of additive capability by technology controlling and process, realizes to containing fibre
The recycling and reuse of dimension element weaving waste resource are controlled to what the efficient quick removal to dyes in dyeing waste water combined with useless
Useless dual purpose.Using cotton fiber as raw material, acrylamide and acrylic acid are monomer, pass through free yl graft polymerization Technology design
The porous cellulose adsorbing material of synthesis.By regulating and controlling the microstructure of adsorbent material and the functional activity group of surface and interface,
Improve its absorption property to dye molecule.
The present invention causes the ratio of free radical, acrylic acid solution, acrylamide and N, the Asia N- by control cellulose and APS
The ratio of bisacrylamide adjusts the surface functional group and absorption property of fiber base aeroge adsorbent obtained.Pass through
N is controlled, the amount of N- methylene-bisacrylamide adjusts the pore structure of porous fibre base aeroge adsorbent, passes through varying functionality
The ratio of monomer realizes the control to functional group, and three-dimensional macroporous structure surface obtained is rich in functions such as hydroxyl, carboxyl and amino
Group.Keep physics, the chemical structure of fiber base aeroge adsorbent to greatest extent by freeze-drying.Frozen dried is in ice
Be lyophilized it is dry during the structure of sample will not be destroyed because solid content is support by the black ice on its seat.In ice
When distillation, hole can be left in dry surplus materials.Thus remain the physics of product and the integrality of chemical structure.
Preferably, further include modified activated carbon in the fiber base aeroge adsorbent, the modified activated carbon and fibre
The mass ratio of dimension element is 0.6~1: 1.
Modified activated carbon is being added in the preparation process of fiber base aeroge adsorbent in the present invention, being capable of reinforcing fiber base
It is rich to enhance its duct for the intensity of aeroge adsorbent.Modified activated carbon is added in cellulose solution, it is made to be uniformly dispersed
After add acrylic acid solution, acrylamide and N, N- methylene-bisacrylamide, so that partial monosomy is passed through in polymerization
Modified activated carbon and fiber base aeroge adsorbent obtained are combined closely in the duct of modified activated carbon, increase fiber base gas
The duct of gel adsorber is rich and intensity.
Preferably, the modified activated carbon the preparation method comprises the following steps: by active carbon be added 8~10M nitric acid solution, activity
Charcoal and the mass volume ratio of nitric acid solution are 1g: 20~40mL, 65~75 DEG C of 9~11h of stirring, 90~110 after filtering, washing
DEG C drying, obtains magnesium oxide/absorbent charcoal.Be added thionyl chloride in obtained magnesium oxide/absorbent charcoal, magnesium oxide/absorbent charcoal and thionyl chloride
Mass ratio is 1: 1.5~3,75~78 DEG C of 3.5~4.5h of reflux, and decompression obtains chlorination modified active carbon after steaming thionyl chloride.
Ethylenediamine is added in chlorination modified active carbon, the mass ratio of chlorination modified active carbon and ethylenediamine is 1: 1.5~3,110~
125 DEG C of 9.5~10.5h of reaction obtain the modified activity of ethylenediamine in 90~110 DEG C of dryings after being washed to neutrality with distillation
Charcoal.
The surface of modified active carbon has amino abundant, can be cross-linked to form hydrogen with the hydroxyl of cellulose surface
Key, when acrylic acid and acrylamide be added carrying out polymerization reaction, further with the carboxyl and amino on acrylic acid and acrylamide
Hydrogen bond is formed, modified activated carbon is fixed in fiber base aeroge adsorbent, and is uniformly dispersed.
Preferably, the degree of neutralization of the acrylic acid is 40~80%.Acrylic acid by being carried out with NaOH to acrylic acid in
With, the degree of neutralization by controlling acrylic acid controls degree of polymerization when acroleic acid polymerization, when the degree of neutralization of acrylic acid is 40~
When 80%, the absorption property of fiber base aeroge adsorbent obtained is good.
Preferably, a kind of preparation method of fiber base aeroge adsorbent the following steps are included:
(1) cellulose is placed in cellulose dissolution liquid after dispersing and is refrigerated to cellulose and is completely dissolved, obtain cellulose solution；
(2) APS is added into cellulose solution and causes free radical, after stirring causes, acrylic acid solution, acrylamide and N is added,
N- methylene-bisacrylamide, stirring polymerization, obtains gelatinous polymer；
(3) gelatinous polymer alcohol and water are cleaned repeatedly, fiber base aeroge adsorbent is obtained after freeze-drying.
The method that the present invention prepares fiber base aeroge adsorbent is simple, easy to operate, and fiber base aeroge obtained is inhaled
Attached dose just has preferable absorption property.
Preferably, a kind of preparation method of fiber base aeroge adsorbent the following steps are included:
(1) cellulose is placed in cellulose dissolution liquid after dispersing and is refrigerated to cellulose and is completely dissolved, obtain cellulose solution；
(2) APS is added into cellulose solution and causes free radical, after stirring causes, modified activated carbon is added, is added third after stirring
Olefin(e) acid solution, acrylamide and N, N- methylene-bisacrylamide, stirring polymerization obtain gelatinous polymer；
(3) gelatinous polymer alcohol and water are cleaned repeatedly, fiber base aeroge adsorbent is obtained after freeze-drying.
Modified activated carbon is added in cellulose solution, acrylic acid solution, acrylamide are added after so that it is uniformly dispersed
And N, N- methylene-bisacrylamide so that partial monosomy polymerization when across the duct of modified activated carbon, by modified active
Charcoal is combined closely with fiber base aeroge adsorbent obtained, and the duct for increasing fiber base aeroge adsorbent is rich and strong
Degree.If modified activated carbon is added together with acrylic acid and acrylamide in the cellulose solution after causing, due to changing after being added
Property active carbon in the evenly dispersed preceding polymer for just having been inserted into cellulose and acrylic acid and acrylamide, modified activated carbon point
Scattered property is poor, and fiber base aeroge adsorbent intensity obtained is poor, easy to break.
Preferably, the mass ratio of the cellulose and cellulose dissolution liquid is 1: 30~35 in step (1)；The fibre
Tie up the mixed liquor that plain lysate is the NaOH solution that concentration is 5~9wt% and the urea liquid that concentration is 10~15wt%；Step
(2) in, the APS causes free radical and cellulose and N, and the mass ratio of N- methylene-bisacrylamide is 1: 10: 0.2~1.
By controlling N, the amount of N- methylene-bisacrylamide adjusts the pore structure of porous fibre base aeroge adsorbent.It is limited in the present invention
Under fixed parameter, fiber base aeroge adsorbent obtained has complicated tridimensional network, to the adsorption energy of dyeing waste-water
Power is stronger.
Preferably, the freezing is in -20~-10 DEG C of 1~3h of freezing in step (1)；In step (2), the stirring
The initiation time is 20~40min；Polymerization temperature is 20~30 DEG C.Fiber base aeroge adsorbent polymeric mild condition of the present invention,
It is easy to operate.
A kind of application of fiber base aeroge adsorbent in dyeing waste-water, the fiber base aeroge adsorbent can with
In TREATMENT OF DYEING WASTEWATER WITH, processing method are as follows: it is 900~1100mg L that fiber base aeroge adsorbent, which is put into concentration,-1Methylene
In base indigo plant solution, 5~120min is adsorbed at room temperature, measures remaining methylene blue count in methylene blue solution.
Fiber base aeroge adsorbent of the invention has stronger adsorption capacity to dyeing waste-water.In a short time
(in 30min) just has preferable adsorption effect.The recycling and reuse to containing cellulose weaving waste resource are realized to dye
The dual purpose for the treatment of wastes with processes of wastes against one another that the efficient quick removal of color Wastewater Dyes combines.
Preferably, the mass volume ratio of the fiber base aeroge adsorbent and methylene blue solution is 0.8~1g:
1mL.The dosage of fiber base aeroge adsorbent of the invention is less, strong to the adsorption capacity of dyeing waste-water.
It is compared with the prior art, the beneficial effects of the present invention are: the present invention is drawn in cellulosic molecule by MOLECULE DESIGN
Enter functional functional group and introduce modified activated carbon in fiber base aeroge adsorbent, by technology controlling and process, obtains to dyeing
Waste water have high efficiency of additive capability cellulose base adsorbent material, realize containing cellulose weaving waste resource recycling and again benefit
Dual purpose.
Detailed description of the invention
Fig. 1 is to be schemed using the SEM of fiber base aeroge adsorbent of the invention；
Fig. 2 is the adsorption effect figure using the fiber base aeroge adsorbent of the embodiment of the present invention 1 to methylene blue.
Specific embodiment
The present invention will be further described with reference to the examples below.Related device, connection structure in the present invention
And method, if being device well known in the art, connection structure and method without refering in particular to.
Embodiment 1
A kind of fiber base aeroge adsorbent, the fiber base aeroge adsorbent is by cellulose, the propylene that degree of neutralization is 60%
Acid and acrylamide are prepared by polymerization reaction, and wherein the mass ratio of cellulose, acrylic acid and acrylamide is 1: 10: 2.
A kind of preparation method of fiber base aeroge adsorbent the following steps are included:
(1) cellulose is placed in cellulose dissolution liquid after dispersing in -15 DEG C of freezing 2h, obtains cellulose solution；Cellulose and fibre
The mass ratio for tieing up plain lysate is 1: 33；The cellulose dissolution liquid is the NaOH solution that concentration is 7wt% and concentration is
The mixed liquor of the urea liquid of 12wt%；
(2) APS is added into cellulose solution and causes free radical, after stirring causes, acrylic acid solution, acrylamide and N is added,
N- methylene-bisacrylamide stirs polyase 13 0min in 25 DEG C, 300rpm, obtains gelatinous polymer；The APS causes certainly
By base and cellulose and N, the mass ratio of N- methylene-bisacrylamide is 1: 10: 0.6；
(3) gelatinous polymer alcohol and water are cleaned repeatedly, obtains fiber base aeroge after -25 DEG C of freeze-drying 20h
Adsorbent.Fig. 2 is the adsorption effect figure using the fiber base aeroge adsorbent of the embodiment of the present invention 1 to methylene blue.Wherein
Before photo B is absorption in figure, picture A is to adsorb after twenty minutes.
A kind of application of fiber base aeroge adsorbent in dyeing waste-water, the fiber base aeroge adsorbent can with
In TREATMENT OF DYEING WASTEWATER WITH, processing method are as follows: it is 1000mg L that fiber base aeroge adsorbent, which is put into concentration,-1Methylene blue it is molten
In liquid, the mass volume ratio of fiber base aeroge adsorbent and methylene blue solution is 0.9g: 1mL, is carried out at room temperature
Absorption measures remaining methylene blue count in methylene blue solution.
Embodiment 1-1
It is 1000mg L by fiber base aeroge adsorbent investment concentration-1Methylene blue solution in, adsorb at room temperature
5min measures remaining methylene blue count in methylene blue solution.
Embodiment 1-2
It is 1000mg L by fiber base aeroge adsorbent investment concentration-1Methylene blue solution in, adsorb at room temperature
10min measures remaining methylene blue count in methylene blue solution.
Embodiment 1-3
It is 1000mg L by fiber base aeroge adsorbent investment concentration-1Methylene blue solution in, adsorb at room temperature
20min measures remaining methylene blue count in methylene blue solution.
Embodiment 1-4
It is 1000mg L by fiber base aeroge adsorbent investment concentration-1Methylene blue solution in, adsorb at room temperature
30min measures remaining methylene blue count in methylene blue solution.
Embodiment 1-5
It is 1000mg L by fiber base aeroge adsorbent investment concentration-1Methylene blue solution in, adsorb at room temperature
60min measures remaining methylene blue count in methylene blue solution.
Embodiment 1-6
It is 1000mg L by fiber base aeroge adsorbent investment concentration-1Methylene blue solution in, adsorb at room temperature
120min measures remaining methylene blue count in methylene blue solution.
Embodiment 2
A kind of fiber base aeroge adsorbent, the fiber base aeroge adsorbent is by cellulose, the propylene that degree of neutralization is 80%
Acid and acrylamide are prepared by polymerization reaction, and wherein the mass ratio of cellulose, acrylic acid and acrylamide is 1: 10: 2.
It further include modified activated carbon in the fiber base aeroge adsorbent, the quality of the modified activated carbon and cellulose
Than being 0.8: 1, the modified activated carbon the preparation method comprises the following steps: active carbon to be added to the nitric acid solution of 9M, active carbon is molten with nitric acid
The mass volume ratio of liquid is 1g: 30mL, 70 DEG C of stirring 10h, in 100 DEG C of dryings after filtering, washing, obtains magnesium oxide/absorbent charcoal.?
Be added thionyl chloride in obtained magnesium oxide/absorbent charcoal, magnesium oxide/absorbent charcoal and thionyl chloride mass ratio be 1: 2,78 DEG C of reflux 4h,
Decompression obtains chlorination modified active carbon after steaming thionyl chloride.Ethylenediamine is added in chlorination modified active carbon, chlorination modified work
Property charcoal and the mass ratio of ethylenediamine be that 1: 2,120 DEG C of reaction 10h in 100 DEG C of dryings after being washed to neutrality with distillation obtain second two
The modified active carbon of amine.
A kind of preparation method of fiber base aeroge adsorbent the following steps are included:
(1) cellulose is placed in cellulose dissolution liquid after dispersing in -15 DEG C of freezing 2h, obtains cellulose solution；Cellulose and fibre
The mass ratio for tieing up plain lysate is 1: 33；The cellulose dissolution liquid is the NaOH solution that concentration is 7wt% and concentration is
The mixed liquor of the urea liquid of 12wt%；
(2) APS is added into cellulose solution and causes free radical, after stirring causes, modified activated carbon is added, is added third after stirring
Olefin(e) acid solution, acrylamide and N, N- methylene-bisacrylamide stir polyase 13 0min in 25 DEG C, 300rpm, obtain gelatinous
Polymer；The APS causes free radical and cellulose and N, and the mass ratio of N- methylene-bisacrylamide is 1: 10: 0.6； (3)
Gelatinous polymer alcohol and water are cleaned repeatedly, obtain fiber base aeroge adsorbent after -25 DEG C of freeze-drying 20h.
A kind of application of fiber base aeroge adsorbent in dyeing waste-water, the fiber base aeroge adsorbent can with
In TREATMENT OF DYEING WASTEWATER WITH, processing method are as follows: it is 1000mg L that fiber base aeroge adsorbent, which is put into concentration,-1Methylene blue it is molten
In liquid, the mass volume ratio of fiber base aeroge adsorbent and methylene blue solution is 0.9g: 1mL, is adsorbed at room temperature
60min measures remaining methylene blue count in methylene blue solution.
Embodiment 3
A kind of fiber base aeroge adsorbent, the fiber base aeroge adsorbent is by cellulose, the propylene that degree of neutralization is 60%
Acid and acrylamide are prepared by polymerization reaction, and wherein the mass ratio of cellulose, acrylic acid and acrylamide is 1: 8: 3.
It further include modified activated carbon in the fiber base aeroge adsorbent, the quality of the modified activated carbon and cellulose
Than being 0.6: 1, the modified activated carbon the preparation method comprises the following steps: active carbon to be added to the nitric acid solution of 10M, active carbon and nitric acid
The mass volume ratio of solution is 1g: 20mL, 75 DEG C of stirring 9h, in 110 DEG C of dryings after filtering, washing, obtains magnesium oxide/absorbent charcoal.?
Be added thionyl chloride in obtained magnesium oxide/absorbent charcoal, magnesium oxide/absorbent charcoal and thionyl chloride mass ratio be 1: 1.5,76 DEG C of reflux
4.5h, decompression obtain chlorination modified active carbon after steaming thionyl chloride.Ethylenediamine is added in chlorination modified active carbon, chlorination changes
Property active carbon and the mass ratio of ethylenediamine be 1: 1.5,125 DEG C of reaction 9.5h, in 110 DEG C of dryings after being washed to neutrality with distillation,
Obtain the modified active carbon of ethylenediamine.
A kind of preparation method of fiber base aeroge adsorbent the following steps are included:
(1) cellulose is placed in cellulose dissolution liquid after dispersing in -20 DEG C of freezing 1h, obtains cellulose solution；Cellulose and fibre
The mass ratio for tieing up plain lysate is 1: 35；The cellulose dissolution liquid is the NaOH solution that concentration is 9wt% and concentration is
The mixed liquor of the urea liquid of 15wt%；
(2) APS is added into cellulose solution and causes free radical, after stirring causes, modified activated carbon is added, is added third after stirring
Olefin(e) acid solution, acrylamide and N, N- methylene-bisacrylamide obtain gelatinous in 30 DEG C, 400rpm stirring polymerization 20min
Polymer；The APS causes free radical and cellulose and N, and the mass ratio of N- methylene-bisacrylamide is 1: 10: 1；
(3) gelatinous polymer alcohol and water are cleaned repeatedly, -20 DEG C of freeze-dryings obtain fiber base aeroge afterwards for 24 hours
Adsorbent.
A kind of application of fiber base aeroge adsorbent in dyeing waste-water, the fiber base aeroge adsorbent can with
In TREATMENT OF DYEING WASTEWATER WITH, processing method are as follows: it is 1100mg L that fiber base aeroge adsorbent, which is put into concentration,-1Methylene blue it is molten
In liquid, the mass volume ratio of fiber base aeroge adsorbent and methylene blue solution is 1g: 1mL, is adsorbed at room temperature
60min measures remaining methylene blue count in methylene blue solution.
Comparative example 1
Comparative example 1 difference from example 1 is that: it is in step (3), gelatinous polymer alcohol and water is repeatedly clear
It washes, is dried at room temperature for obtaining fiber base aeroge adsorbent afterwards for 24 hours.Other are same as Example 1.
Comparative example 2
Comparative example 2 difference from example 1 is that: use degree of neutralization for 38% acrylic acid solution prepare fiber base airsetting
Glue adsorbent.Other are same as Example 1.
Comparative example 3
Comparative example 3 difference from example 1 is that: in step (2), APS cause free radical, acrylic acid solution, acryloyl
Amine, modified activated carbon and N, the mass ratio of N- methylene-bisacrylamide are 1: 122: 8: 0.6,.Other with 1 phase of embodiment
Together.
Comparative example 4
Comparative example 4 and embodiment 2 the difference is that: in step (2), APS is added into cellulose solution and causes free radical,
After stirring causes 30min, acrylic acid solution, acrylamide, modified activated carbon and N that degree of neutralization is 60%, N- methylene is added
Bisacrylamide.Other are same as Example 2.
Comparative example 5
Comparative example 5 and embodiment 2 the difference is that: in step (2), replace modified activated carbon with active carbon.Other with
Embodiment 2 is identical.
It is real that methylene blue adsorption number is carried out using fiber base aeroge adsorbent made from Examples 1 to 3 and comparative example 1~5
It tests, detects the adsorbance when adsorbing 60min of fiber base aeroge adsorbent obtained.Testing result is shown in Table 1.
The calculation method of adsorbance are as follows: qe=(c0-ct)×V/m；In formula, qeIt is sample to the adsorbance of dye molecule, it is single
Position g g-1；c0For the initial concentration of dyestuff, unit g L-1；ctFor the concentration of dye molecule in the adsorbent solution at the sampling moment,
Unit g L-1；M is the quality of adsorbent, and unit g, V are the volume of solution, unit L.
Table 1
| Group number | Adsorbance (g/g) |
| Embodiment 1 | 775 |
| Embodiment 2 | 786 |
| Embodiment 3 | 785 |
| Comparative example 1 | 732 |
| Comparative example 2 | 740 |
| Comparative example 3 | 743 |
| Comparative example 4 | 730 |
| Comparative example 5 | 725 |
As can be seen from Table 1, adsorptivity of the fiber base aeroge adsorbent made from method of the invention to methylene blue dye
It can be good.After comparative example 1 replaces freeze-drying with common drying means, fiber base aeroge adsorbent obtained is to methylene
The absorption property of blue dyestuff is decreased obviously.Comparative example 2 prepares fiber base aeroge using the acrylic acid solution that degree of neutralization is 38%
Adsorbent, the absorption property and embodiment 1 of fiber base aeroge adsorbent obtained have significant difference, it was demonstrated that acrylic acid solution
Degree of neutralization on result influence it is fairly obvious, not being can be optional.Comparative example 3 changes acrylic acid and acrylamide
Ratio makes it beyond restriction range of the invention, the adsorption capacity and 1 difference of embodiment of fiber base aeroge adsorbent obtained
Obviously.Comparative example 4 changes the addition sequence of modified activated carbon, by modified activated carbon and acrylic acid solution, acrylamide and N,
N- methylene-bisacrylamide is added in cellulose solution together, prepares fiber base aeroge adsorbent, and absorption property is more real
Example 2 is applied to be decreased obviously.Comparative example 5 replaces modified activated carbon, the adsorptivity of fiber base aeroge adsorbent obtained with active carbon
It can be decreased obviously compared with embodiment 2.Illustrate that only absorption property could be obtained using method and technological parameter of the invention good
Fiber base aeroge adsorbent.
The above is only the preferred embodiment of invention, is not intended to limit the invention in any way, all skills according to the present invention
Art any simple modification, change and equivalent structure transformation substantially to the above embodiments, still fall within the technology of the present invention
The protection scope of scheme.
Claims (10)
1. a kind of fiber base aeroge adsorbent, it is characterised in that: the fiber base aeroge adsorbent is by cellulose, acrylic acid
Be prepared with acrylamide by polymerization reaction, wherein the mass ratio of cellulose, acrylic acid and acrylamide be 1:8 ~ 12:1 ~
3。
2. a kind of fiber base aeroge adsorbent as described in claim 1, it is characterised in that: the fiber base aeroge absorption
It further include modified activated carbon in agent, the mass ratio of the modified activated carbon and cellulose is 0.6 ~ 1:1.
3. a kind of fiber base aeroge adsorbent as claimed in claim 2, it is characterised in that: the preparation of the modified activated carbon
Method are as follows: by the nitric acid solution of 8 ~ 10M of active carbon addition, the mass volume ratio of active carbon and nitric acid solution is 1g:20 ~ 40mL,
65 ~ 75 DEG C of 9 ~ 11h of stirring obtain magnesium oxide/absorbent charcoal in 90 ~ 110 DEG C of dryings after filtering, washing；In obtained magnesium oxide/absorbent charcoal
Middle addition thionyl chloride, magnesium oxide/absorbent charcoal and thionyl chloride mass ratio be 1:1.5 ~ 3,75 ~ 78 DEG C of 3.5 ~ 4.5h of reflux, depressurize
Chlorination modified active carbon is obtained after steaming thionyl chloride；Ethylenediamine is added in chlorination modified active carbon, chlorination modified active carbon
Mass ratio with ethylenediamine is 1:1.5 ~ 3, in 110 ~ 125 DEG C of 9.5 ~ 10.5h of reaction, 90 ~ 110 after being washed to neutrality with distillation
DEG C drying obtains the modified active carbon of ethylenediamine.
4. a kind of fiber base aeroge adsorbent as claimed in claim 1 or 2, it is characterised in that: the neutralization of the acrylic acid
Degree is 40 ~ 80%.
5. a kind of fiber base aeroge adsorbent as described in claim 1 is any, it is characterised in that preparation method include with
Lower step:
(1) cellulose is placed in cellulose dissolution liquid after dispersing and is refrigerated to cellulose and is completely dissolved, obtain cellulose solution；
(2) APS is added into cellulose solution and causes free radical, after stirring causes, acrylic acid solution, acrylamide and N is added,
N- methylene-bisacrylamide, stirring polymerization, obtains gelatinous polymer；
(3) gelatinous polymer alcohol and water are cleaned repeatedly, fiber base aeroge adsorbent is obtained after freeze-drying.
6. a kind of fiber base aeroge adsorbent as described in claim 2 is any, it is characterised in that preparation method include with
Lower step:
(1) cellulose is placed in cellulose dissolution liquid after dispersing and is refrigerated to cellulose and is completely dissolved, obtain cellulose solution；
(2) APS is added into cellulose solution and causes free radical, after stirring causes, modified activated carbon is added, is added third after stirring
Olefin(e) acid solution, acrylamide and N, N- methylene-bisacrylamide, stirring polymerization obtain gelatinous polymer；
(3) gelatinous polymer alcohol and water are cleaned repeatedly, fiber base aeroge adsorbent is obtained after freeze-drying.
7. such as a kind of fiber base aeroge adsorbent described in claim 5 or 6, it is characterised in that: in step (1), the fibre
The mass ratio of dimension element and cellulose dissolution liquid is 1:30 ~ 35；The cellulose dissolution liquid is the NaOH solution that concentration is 5 ~ 9wt%
With the mixed liquor for the urea liquid that concentration is 10 ~ 15wt%；In step (2), the APS causes free radical and cellulose and N, N-
The mass ratio of methylene-bisacrylamide is 1:10:0.2 ~ 1.
8. a kind of fiber base aeroge adsorbent as claimed in claim 7, it is characterised in that: in step (1), the freezing is
In -20 ~ -10 DEG C of 1 ~ 3h of freezing；In step (2), the stirring causes the time as 20 ~ 40min；Polymerization temperature is 20 ~ 30 DEG C.
9. a kind of application of the fiber base aeroge adsorbent in dyeing waste-water as described in claim 5 or 6 is any, feature
Be: the fiber base aeroge adsorbent can with for TREATMENT OF DYEING WASTEWATER WITH, processing method are as follows: adsorb fiber base aeroge
It is 900 ~ 1100mg L that agent, which puts into concentration,-1Methylene blue solution in, at room temperature adsorb 5 ~ 120min, measure methylene
Remaining methylene blue count in blue solution.
10. a kind of application of the fiber base aeroge adsorbent as claimed in claim 9 in dyeing waste-water, it is characterised in that:
The mass volume ratio of the fiber base aeroge adsorbent and methylene blue solution is 0.8 ~ 1g:1mL.
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