CN108421535A - A kind of method of cellulose/hectorite hybrid composite material purification organic wastewater containing phenol - Google Patents
A kind of method of cellulose/hectorite hybrid composite material purification organic wastewater containing phenol Download PDFInfo
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- CN108421535A CN108421535A CN201810536748.1A CN201810536748A CN108421535A CN 108421535 A CN108421535 A CN 108421535A CN 201810536748 A CN201810536748 A CN 201810536748A CN 108421535 A CN108421535 A CN 108421535A
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- hectorite
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- cellulose acetate
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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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- 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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
Abstract
The invention belongs to water pollution control technology fields, and in particular to a kind of method of cellulose/hectorite hybrid composite material purification organic wastewater containing phenol.The ultrasonic hydridization in the aqueous solution of ethyl alcohol forms the cellulose acetate phthalate that cellulose of the present invention/hectorite hybrid composite material is grafted by 2 acrylamide, 2 methyl propane sulfonic acid with hectorite.Cellulose of the present invention/hectorite hybrid composite material can be used for removing the substance containing phenol in organic wastewater, is significantly larger than conventional carbon to the removal rate height and adsorbance of the substance containing phenol, has industrial applications foreground.
Description
Technical field
The invention belongs to water pollution control technology fields, and in particular to a kind of cellulose/hectorite hybrid composite material is net
Change the method for the organic wastewater containing phenol.
Background technology
With industrial boom, the type and quantity of waste water rapidly increase, also increasingly extensively and tight to the pollution of water body
Weight, threatens the health and safety of the mankind.There are many high concentrated organic wastewater type, as coking wastewater, pharmacy waste water, weaving/, printing and dyeing
Waste water, oil/wastewater from chemical industry etc..Arylamine, phenol, the homologue of phenol and naphthalene, anthracene, BaP etc. are usually contained in pharmacy waste water
Polycyclic compound and cyanide, sulfide, rhodanide etc..
Phenol wastewater is typical a kind of organic wastewater, because it causes aquatile mortality, inhibits micropopulation
Fall, cause animal carcinogenic etc., so the discharge standard of phenol wastewater is very strict at present, municipal wastewater treatment plant is discharged into the water of surface water
Provide that volatile phenol content is less than 0.5mg/L in matter standard.There are extraction, chemical oxidation to the processing mode of phenol wastewater at present
Method, chemical precipitation method, physisorphtion, electrolysis, biochemical process etc..Wherein physisorphtion research and application are more, especially
Using activated carbon, to adsorb phenol wastewater, (chemical industry is in progress, 2018,37 (2)：744-751, activated carbon adsorption Phenol-Containing Wastewater Treatment
Progress), but due to the source of activated carbon difference so that its performance difference is larger；And activated carbon is to phenol wastewater
Adsorbance is often smaller.
Cellulose is a kind of most abundant in the world renewable macromolecule natural resources, cellulose and hemicellulose, wooden
Element by combine or quasi integration in a manner of be present in plant cell.Due between cellulosic molecule because hydroxyl hydrogen bond action and
With very strong interaction force, and on cellulose molecular chain there is great amount of hydroxy group to exist, so cellulose is with stronger
Reactivity.
Hectorite also known as lithium magnesium silicate are non-metal composite nano materials.Lithium magnesium silicate, that is, hectorite is important smectite
One of class mineral have 2：1 type layered crystal structure.It has excellent hydrophilic swelling and suspension thixotropy, can be in water
Disperse well.
Waste water is handled using cellulose although having been had been reported that in currently available technology, as disclosed in CN104710038A
A kind of method using cellulose base flocculant coagulation decoloration dyeing waste water, but it has functioned only as absorption coloring matter
Effect, i.e. chroma removal rate achieve good result, but for that can solve colourless substance in waste water, such as aldehydes matter.
Document report is had no to remove the substance containing phenol in organic wastewater using hectorite and cellulose composite hybridization.
Invention content
The object of the present invention is to provide a kind of composite materials using cellulose/hectorite hydridization to remove in organic sewage
Substance containing phenol, the present invention carries out hybridization compounding with hectorite and the cellulose acetate phthalate of graft modification and prepares fiber
The composite material for tieing up element/hectorite hydridization can be used for removing the substance containing phenol in organic wastewater, to the removal rate of the substance containing phenol
High and adsorbance is significantly larger than conventional carbon, has industrial applications foreground.
According to the first aspect of the invention, the present invention provides a kind of systems of cellulose/hectorite hybrid composite material
Preparation Method, acetic acid neighbour's benzene that the cellulose/hectorite hybrid composite material is grafted by 2- acrylamide -2- methyl propane sulfonic acids
The ultrasonic hydridization in the aqueous solution of ethyl alcohol forms diformazan acid cellulose with hectorite.
The preparation method of cellulose according to the present invention/hectorite hybrid composite material, the specific steps are：
1) preparation of hectorite nano material：
Magnesium hydroxide 1-A) is added in lithium fluoride aqueous solution, stirring 2-3h obtains the first mixed liquor at 40-50 DEG C；
1-B) the first mixed liquor is added drop-wise in Ludox, homogeneous mixture is stirred at 35-40 DEG C, then temperature rising reflux
Reaction 16-18h obtains hectorite dispersion liquid；
Hectorite dispersion liquid 1-C) is cooled to room temperature, is centrifuged, filter cake is collected and is placed in the toluene solution of 0.5%V oleic acid,
Ultrasonic disperse 1-2 days at 80-90 DEG C, cooling, centrifugation, collect filter cake under air atmosphere with the heating rate of 5 DEG C/min
It is warming up to 150-180 DEG C, last heat preservation and dryness 5-6h obtains hectorite nano material；
The present invention (i.e. obtained by step 1-B) by aqueous solution treated hectorite in order to be prepared into the nanometer of high degree of dispersion
Grain, increases toluene ultrasonic disperse treatment process, and contains a small amount of oleic acid in toluene, is in order to avoid water that ultrasonic disperse is opened
Pyroxene occurs to reunite or gather, and influences the hectorite appearance of nano material finally prepared；
2) preparation of the cellulose acetate phthalate of 2- acrylamides -2- methyl propane sulfonic acids grafting：
100g cellulose acetate phthalates 2-A) are configured to the aqueous dispersions of 5-8%wt with deionized water, then
Cellulosic acidic solution is obtained using hydrochloric acid regulation system pH to 2.0；Cellulose acetate phthalate is compared compared with traditional fibre element
Containing phenyl ring, it is conducive to compatible with useless Organic substance in water, increases its removal efficiency to organic matter；
0.5g initiator ammonium ceric nitrate stirring and dissolvings 2-B) are added into cellulosic acidic solution, are warming up to 50-60 DEG C,
300-400mmol2- acrylamide -2- methyl propane sulfonic acid insulated and stirreds 1-2h is added under nitrogen atmosphere and obtains 2- acrylamides -2-
The cellulose acetate phthalate dispersion liquid of methyl propane sulfonic acid grafting；Cellulose acetate phthalate in acid condition
The fracture of oxygen bridge key hydrolyze, the exposed hydroxyl of fracture generation polymerize with 2- acrylamide -2- methyl propane sulfonic acids；
2-C) the cellulose acetate phthalate dispersion liquid by the grafting of 2- acrylamide -2- methyl propane sulfonic acids centrifuges,
Filter cake is washed to filtrate into neutrality, then collects filter cake and is dried under vacuum to constant weight at 50-60 DEG C and obtains 2- acrylamide -2- methyl
The cellulose acetate phthalate of propane sulfonic acid grafting；
3) preparation of cellulose/hectorite hybrid composite material
By the cellulose acetate phthalate ultrasonic disperse of 2- acrylamide -2- methyl propane sulfonic acids grafting in 80%V
Ethanol water in, ultrasound 1-2 days at 40-50 DEG C of hectorite nano material are then added, centrifugation, is collected and filtered at filter cake washing
Cake is dried to constant weight at 45 DEG C and obtains cellulose/hectorite hybrid composite material.
Preferably, by weight calculating, the acetic acid neighbour benzene two of 2- acrylamide -2- methyl propane sulfonic acids grafting in step 3)
Cellulose formiate：Hectorite nano material=1:30-60；Further preferably 1:40.
Preferably, step 1-B) in calculated according to molar ratio, lithium fluoride:Magnesium hydroxide:Silica=1:4:8；It is described
Ludox is the dispersion liquid of nanometer silicon dioxide particle in water, and the weight percent of silica is 20% in dispersion liquid.
According to another aspect of the present invention, the present invention provides a kind of use of cellulose/hectorite hybrid composite material
On the way, it is used for adsorption cleaning organic wastewater.
Preferably, the organic wastewater is phenol wastewater, and the further phenol wastewater is phenolic waste water, p-nitrophenyl
One or more kinds of mixing of phenol waste water, parachlorophenol waste water, para-aminophenol, further preferably p-nitrophenol or
Para-aminophenol.
The present invention has the advantages that：
1) it is miscellaneous using the cellulose of graft modification with hectorite to prepare a kind of novel cellulose/hectorite as raw material by the present invention
Change composite material；
2) cellulose/hectorite hybrid composite material prepared by the present invention can be used for adsorption cleaning organic wastewater, especially
Substance containing phenol in waste water；
3) cellulose/hectorite hybrid composite material prepared by the present invention is high to the removal rate and adsorbance of phenol wastewater,
When in particular by cellulose acetate phthalate being raw material, to the removal rate of phenol wastewater higher than the preparation of traditional fibre element
Hybrid composite material；
4) present invention increases ultrasonic process in the toluene solution of oleic acid when preparing hectorite, overcomes hectorite
The defect that nano material is easily reunited；
5) since hectorite can be uniformly dispersed in water phase, so hybridization compounding is carried out using hectorite and cellulose,
Keep the composite material prepared fully dispersed in water；
6) cellulose acetate phthalate that hectorite is grafted with 2- acrylamide -2- methyl propane sulfonic acids is in organic waste
There is certain synergistic function in terms of Water warfare.
Specific implementation mode
In order to make the objectives, technical solutions and advantages of the present invention clearer, With reference to embodiment, to this
Invention is further described.It should be understood that these descriptions are merely illustrative, and it is not intended to limit the scope of the present invention.
Raw material：Cellulose acetate phthalate comes from Sigma-Aldrich (Shanghai) trade Co., Ltd, product
Article No. is 22192, molecular weight 2534.12g/mol；Cocoanut active charcoal (comes from traditional Chinese medicines chemical reagent, product identification
10006755,200 mesh of grain size)；Remaining raw material is commercially available convenient source.
To simulate the removal effect of the organic wastewater containing phenol, phenol-water solution is made by oneself as follows：
Take substance containing phenol in conical flask, with the H of 0.1mol/L2SO4Or 0.1mol/L NaOH aqueous solutions adjust pH value of solution
Value, is added a certain amount of adsorbent, conical flask is put into 40 DEG C of thermostatic control oscillator vibrations, rotating speed of the control temperature in 200r/min
It is filtered after lower stirring 12h, using the concentration of HPLC external standard methods substance containing phenol.
One, the Q of species adsorption containing phenolm(mg/g) formula (1) is shown in measurement：
In formula, C0And CtThe concentration of the substance containing phenol when respectively initial and adsorption equilibrium in solution, mg/L；V is solution body
Product, L；M is quantity of sorbent, g.Test method measurement method with reference to as defined in standard GB/T/T 7702.8-2008.
Two, the detection method of the removal rate of substance containing phenol R：
The removal rate R (%) of the substance containing phenol is calculated with formula (2) in aqueous solution：
In formula, C0It is respectively the concentration of amount of substance containing phenol in initial and filtrate, mg/L with C.
Embodiment 1
1) preparation of hectorite nano material：
1-A) 100mmol lithium fluoride is dissolved in 200ml water, and the magnesium hydroxide of 400mmol is then added, is stirred at 40-50 DEG C
It mixes 2-3h and obtains the first mixed liquor；
1-B) the first mixed liquor is added drop-wise in Ludox (for the SiO of 20%wt2Aqueous dispersions, SiO in aqueous dispersions2
Mole be 800mmol), stir into homogeneous mixture at 35-40 DEG C, then temperature rising reflux reaction 16-18h obtains hectorite point
Dispersion liquid；
Hectorite dispersion liquid 1-C) is cooled to room temperature, is centrifuged, filter cake is collected and is placed in the toluene solution of 0.5%V oleic acid,
Ultrasonic disperse 1-2 days at 80-90 DEG C, cooling, centrifugation, collect filter cake under air atmosphere with the heating rate of 5 DEG C/min
It is warming up to 150-180 DEG C, last heat preservation and dryness 5-6h obtains hectorite nano material (hectorite nano material is abbreviated as NanoH)；
2) preparation of the cellulose acetate phthalate of 2- acrylamides -2- methyl propane sulfonic acids grafting：
100g cellulose acetate phthalates 2-A) are configured to the aqueous dispersions of 6%wt with deionized water, are then adopted
Cellulosic acidic solution is obtained with hydrochloric acid regulation system pH to 2.0；
0.5g initiator ammonium ceric nitrate stirring and dissolvings 2-B) are added into cellulosic acidic solution, are warming up to 50-60 DEG C,
360mmol 2- acrylamide -2- methyl propane sulfonic acid insulated and stirreds 1-2h is added under nitrogen atmosphere and obtains 2- acrylamide -2- first
The cellulose acetate phthalate dispersion liquid of base propane sulfonic acid grafting；
2-C) the cellulose acetate phthalate dispersion liquid by the grafting of 2- acrylamide -2- methyl propane sulfonic acids centrifuges,
Filter cake is washed to filtrate into neutrality, then collects filter cake and is dried under vacuum to constant weight at 50-60 DEG C and obtains 2- acrylamide -2- methyl
Cellulose acetate phthalate (the acetic acid neighbour benzene two of 2- acrylamide -2- methyl propane sulfonic acids grafting of propane sulfonic acid grafting
Cellulose formiate is abbreviated as AC)；
3) preparation of cellulose/hectorite hybrid composite material
The cellulose acetate phthalate ultrasonic disperse that 1.0g 2- acrylamide -2- methyl propane sulfonic acids are grafted is existed
In the ethanol water of 200ml 80%V, ultrasound 2 days at 40-50 DEG C of 40.0g hectorites nano material, centrifugation, filter is then added
Cake washing is collected filter cake and is dried at 45 DEG C and to constant weight obtains cellulose/hectorite hybrid composite material (cellulose/hectorite is miscellaneous
Change composite material and be abbreviated as AC/H).
Embodiment 1-A
Cellulose acetate phthalate in embodiment 1 is replaced by by cellulose acetate using single-factor variable method, i.e.,
Compared with Example 1, using etc. the cellulose acetates of weight replace cellulose acetate phthalate, remaining and embodiment 1
Preparation method is completely the same.The cellulose prepared/hectorite hybrid composite material is defined as C/H.
Embodiment 2
Hectorite nano material (NanoH), the 2- acrylamide -2- methyl propane sulfonic acids prepared to embodiment 1 is grafted
Cellulose acetate phthalate (AC), cellulose/hectorite hybrid composite material (AC/H) and C/H are adsorbent in different pH
Removal rate R (the initial phenol concentration C of its Pyrogentisinic Acid are measured under value0Additive amount for 50mg/L, adsorbent is 40mg/L), knot
Fruit is as shown in table 1：
The removal rate R of the different adsorbent Pyrogentisinic Acids at pH of table 1
Note："-" representative is not tested；Front.Environ.Sci.Eng.2013,7(2):158–165,Removal
Report cocoanut active charcoal in pH=9.0 items in of phenol by powdered activated carbon adsorption
There is maximum adsorption activity, so not carrying out the experiment under the conditions of other pH under part.
The above result shows that cellulose/hectorite hybrid composite material (AC/H) Pyrogentisinic Acid prepared by the present invention has relatively by force
Adsorption cleaning effect, hectorite and 2- acrylamide -2- methyl propane sulfonic acids grafting cellulose acetate phthalate tool
There is certain synergy, and the suction-operated of its Pyrogentisinic Acid is significantly larger than cocoanut active charcoal.
Embodiment 3
Cellulose/hectorite the hybrid composite material (AC/H) prepared with embodiment 1 is that adsorbent is surveyed at various ph values
Measure its removal rate R (initial concentration C of the substance containing phenol to difference substance containing phenol0Additive amount for 50mg/L, adsorbent is
40mg/L), the results are shown in Table 2：
The removal rate R of difference substance containing phenol under the different pH value of table 2
The above test results show that cellulose/hectorite hybrid composite material (AC/H) prepared by the present invention is for major part
Substance containing phenol all has excellent Adsorption effect, especially p-nitrophenol and para-aminophenol, in wider pH models
Excellent absorption property is all had in enclosing, actual industrial is facilitated to handle.
Embodiment 4
With embodiment 1 prepare cellulose/hectorite hybrid composite material (AC/H) be adsorbent respectively substance containing phenol most
Its corresponding adsorbance Q is measured under excellent absorption pH valuem(the initial concentration C of the substance containing phenol0For 50mg/L), result such as 3 institute of table
Show：
The adsorbance Q of the different phenol wastewater of table 3m
| Substance containing phenol | Phenol | P-nitrophenol | Parachlorophenol | Para-aminophenol | Catechol |
| pH | 6.0 | 6.0 | 7.0 | 8.0 | 7.0 |
| Qm(mg/g) | 268.6 | 379.9 | 198.2 | 296.4 | 334.2 |
The above result shows that cellulose/hectorite hybrid composite material (AC/H) prepared by the present invention is to different objects containing phenol
The adsorbance Q of mattermDifference, with the adsorbance maximum of p-nitrophenol, far superior to conventional wooden activated carbon.
Although embodiments of the present invention are described in detail, it should be understood that, without departing from the present invention's
In the case of spirit and scope, can embodiments of the present invention be made with various changes, replacement and change.
Claims (8)
1. a kind of preparation method of cellulose/hectorite hybrid composite material, it is characterised in that：Cellulose/the hectorite is miscellaneous
The cellulose acetate phthalate that change composite material is grafted by 2- acrylamide -2- methyl propane sulfonic acids is with hectorite in ethyl alcohol
Aqueous solution in ultrasonic hydridization form.
2. preparation method according to claim 1, it is characterised in that：Specifically comprise the following steps：
1）The preparation of hectorite nano material：
1-A）Magnesium hydroxide is added in lithium fluoride aqueous solution, stirring 2-3h obtains the first mixed liquor at 40-50 DEG C；
1-B）First mixed liquor is added drop-wise in Ludox, homogeneous mixture is stirred at 35-40 DEG C, then temperature rising reflux reacts
16-18h obtains hectorite dispersion liquid；
Hectorite dispersion liquid 1-C) is cooled to room temperature, is centrifuged, filter cake is collected and is placed in the toluene solution of 0.5%V oleic acid, in 80-
Ultrasonic disperse 1-2 days at 90 DEG C, cooling, centrifugation collect filter cake in being warming up to the heating rate of 5 DEG C/min under air atmosphere
150-180 DEG C, last heat preservation and dryness 5-6h obtains hectorite nano material；
2）The preparation of the cellulose acetate phthalate of 2- acrylamide -2- methyl propane sulfonic acids grafting：
2-A）100g cellulose acetate phthalates are configured to the aqueous dispersions of 5-8%wt with deionized water, then use salt
Sour regulation system pH to 2.0 obtains cellulosic acidic solution；
2-B）0.5g initiator ammonium ceric nitrate stirring and dissolvings are added into cellulosic acidic solution, 50-60 DEG C are warming up to, in nitrogen
300-400mmol 2- acrylamide -2- methyl propane sulfonic acid insulated and stirreds 1-2h is added under atmosphere and obtains 2- acrylamide -2- first
The cellulose acetate phthalate dispersion liquid of base propane sulfonic acid grafting；
2-C）By the cellulose acetate phthalate dispersion liquid centrifugation of 2- acrylamide -2- methyl propane sulfonic acids grafting, filter cake
Filtrate is washed into neutrality, filter cake is then collected and is dried under vacuum to constant weight at 50-60 DEG C and obtain 2- acrylamide -2- methylpropanes
The cellulose acetate phthalate of Sulphonic Acid Functionalized；
3）The preparation of cellulose/hectorite hybrid composite material：
Ethyl alcohol of the cellulose acetate phthalate ultrasonic disperse that 2- acrylamide -2- methyl propane sulfonic acids are grafted in 80%V
In aqueous solution, ultrasound 1-2 days at 40-50 DEG C of hectorite nano material are then added, centrifugation, collects filter cake in 45 at filter cake washing
It is dried to constant weight at DEG C and obtains cellulose/hectorite hybrid composite material.
3. preparation method according to claim 2, it is characterised in that：Step 3）In by weight calculate, 2- acrylamides-
The cellulose acetate phthalate of 2- methyl propane sulfonic acids grafting：Hectorite nano material=1:30-60.
4. preparation method according to claim 2, it is characterised in that：Step 1-B）In calculated according to molar ratio, lithium fluoride:
Magnesium hydroxide:Silica=1:4:8；The Ludox is the dispersion liquid of nanometer silicon dioxide particle in water, two in dispersion liquid
The weight percent of silica is 20%.
5. a kind of purposes of any one of claim 1-4 celluloses/hectorite hybrid composite material, it is characterised in that：With
In adsorption cleaning organic wastewater.
6. purposes according to claim 5, it is characterised in that：The organic wastewater is phenol wastewater.
7. purposes according to claim 6, it is characterised in that：The phenol wastewater is phenolic waste water, p-nitrophenol is useless
One or more kinds of mixing of water, parachlorophenol waste water, para-aminophenol.
8. purposes according to claim 6, it is characterised in that：The phenol wastewater is p-nitrophenol or p-aminophenyl
Phenol.
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Cited By (1)
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| CN110918061A (en) * | 2019-12-17 | 2020-03-27 | 甘肃农业大学 | Biomass waste activated carbon, preparation method thereof and application of biomass waste activated carbon in treatment of nitrophenol compounds in wastewater |
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