CN108421535B - Method for purifying phenol-containing organic wastewater by using cellulose/hectorite hybrid composite material - Google Patents
Method for purifying phenol-containing organic wastewater by using cellulose/hectorite hybrid composite material Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- C02F1/28—Treatment of water, waste water, or sewage by sorption
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Abstract
The invention belongs to the technical field of water pollution control, and particularly relates to a method for purifying phenol-containing organic wastewater by using a cellulose/hectorite hybrid composite material. The cellulose/hectorite hybrid composite material is prepared by carrying out ultrasonic hybridization on 2-acrylamide-2-methylpropanesulfonic acid grafted cellulose acetate phthalate and hectorite in an ethanol water solution. The cellulose/hectorite hybrid composite material can be used for removing phenol-containing substances in organic wastewater, has high removal rate of the phenol-containing substances and far higher adsorption capacity than that of the traditional activated carbon, and has industrial application prospect.
Description
Technical Field
The invention belongs to the technical field of water pollution control, and particularly relates to a method for purifying phenol-containing organic wastewater by using a cellulose/hectorite hybrid composite material.
Background
With the rapid development of industry, the variety and quantity of waste water are rapidly increased, the pollution to water is becoming wide and serious, and the health and safety of human beings are threatened. The high-concentration organic wastewater is of various types, such as coking wastewater, pharmaceutical wastewater, textile wastewater, printing wastewater, petroleum/chemical wastewater and the like. Pharmaceutical wastewater generally contains aromatic amine, phenol, and homologues of phenol, polycyclic compounds such as naphthalene, anthracene, benzopyrene, etc., and cyanide, sulfide, thiocyanide, etc.
Phenolic wastewater is a typical organic wastewater, and because it causes massive death of aquatic organisms, inhibits microbial communities, causes carcinogenesis of animals and the like, the discharge standard of phenolic wastewater is very strict at present, and the volatile phenol content is regulated to be lower than 0.5mg/L in the water quality standard of surface water discharged by municipal sewage plants. At present, the phenolic wastewater is treated by extraction method, chemical oxidation method, chemical precipitation method, physical adsorption method, electrolysis method, biochemical method and the like. The physical adsorption method has more researches and applications, particularly, the activated carbon is adopted to adsorb the phenol-containing wastewater (the chemical engineering progresses, 2018,37 (2): 744-751), and the research progress of the activated carbon adsorption treatment of the phenol-containing wastewater is advanced), but the source of the activated carbon is different, so that the performance difference is larger; and the adsorption capacity of the activated carbon to the phenol-containing wastewater is usually small.
Cellulose is the most abundant renewable high molecular natural resource in the world, and the cellulose, hemicellulose and lignin exist in plant cells in a combined or semi-combined mode. Cellulose has strong interaction force because of hydrogen bond action of hydroxyl, and a large amount of hydroxyl exists on a cellulose molecular chain, so that the cellulose has strong reaction activity.
Hectorite, also known as lithium magnesium silicate, is a non-metallic composite nanomaterial. Lithium magnesium silicate, hectorite, is one of the important smectite minerals, having a weight ratio of 2: layer 1 type layered crystal structure. It has excellent hydrophilic swelling property and suspended thixotropy, and can be well dispersed in water.
Although the prior art reports that cellulose is used for treating wastewater, for example, CN104710038A discloses a method for coagulating and decolorizing printing and dyeing wastewater by using cellulose-based flocculant, it only plays a role of adsorbing colored substances, i.e., the removal rate of chromaticity is good, but the problem of colorless substances in wastewater, such as phenolic substances, is solved.
The method for removing phenol-containing substances in organic wastewater by adopting composite hybridization of hectorite and cellulose is not reported in documents.
Disclosure of Invention
The invention aims to provide a method for removing phenol-containing substances in organic sewage by adopting a cellulose/hectorite hybrid composite material.
According to a first aspect of the invention, the invention provides a preparation method of a cellulose/hectorite hybrid composite material, wherein the cellulose/hectorite hybrid composite material is formed by carrying out ultrasonic hybridization on cellulose acetate phthalate grafted by 2-acrylamide-2-methylpropanesulfonic acid and hectorite in an aqueous solution of ethanol.
The preparation method of the cellulose/hectorite hybrid composite material comprises the following specific steps:
1) preparing a hectorite nano material:
1-A) adding magnesium hydroxide into a lithium fluoride aqueous solution, and stirring for 2-3h at 40-50 ℃ to obtain a first mixed solution;
1-B) dropwise adding the first mixed solution into silica sol, stirring at 35-40 ℃ to obtain a uniform mixture, and then heating for reflux reaction for 16-18h to obtain a hectorite dispersion solution;
1-C) cooling the hectorite dispersion liquid to room temperature, centrifuging, collecting filter cakes, placing the filter cakes in a toluene solution of 0.5% V oleic acid, performing ultrasonic dispersion for 1-2 days at the temperature of 80-90 ℃, cooling, centrifuging, collecting the filter cakes, heating to 180 ℃ at the heating rate of 5 ℃/min in the air atmosphere, and finally performing heat preservation and drying for 5-6h to obtain the hectorite nano material;
in order to prepare the hectorite (obtained in the step 1-B) treated by the aqueous solution into highly dispersed nano particles, the invention adds a toluene ultrasonic dispersion treatment process, and the toluene contains a small amount of oleic acid, so that the phenomenon that the hectorite dispersed by ultrasonic is agglomerated or accumulated to influence the morphology of the finally prepared hectorite nano material is avoided;
2) preparation of 2-acrylamido-2-methylpropanesulfonic acid grafted cellulose acetate phthalate:
2-A) preparing 100g of cellulose acetate phthalate into 5-8 wt% of aqueous dispersion by using deionized water, and then adjusting the pH of the system to 2.0 by using hydrochloric acid to obtain cellulose acidic solution; compared with the traditional cellulose, the cellulose acetate phthalate contains benzene rings, is beneficial to being compatible with organic matters in the wastewater, and increases the removal efficiency of the organic matters;
2-B) adding 0.5g of initiator ammonium ceric nitrate into the cellulose acidic solution, stirring and dissolving, heating to 50-60 ℃, adding 300-400mmol 2-acrylamide-2-methylpropanesulfonic acid under nitrogen atmosphere, keeping the temperature and stirring for 1-2h to obtain 2-acrylamide-2-methylpropanesulfonic acid grafted cellulose acetate phthalate dispersion liquid; under the acidic condition, the oxygen bridge bond of the cellulose acetate phthalate is broken to generate hydrolysis, and the broken exposed hydroxyl is polymerized with 2-acrylamide-2-methylpropanesulfonic acid;
2-C) centrifuging the 2-acrylamide-2-methylpropanesulfonic acid grafted cellulose acetate phthalate dispersion, washing a filter cake with water until the filtrate becomes neutral, collecting the filter cake, and drying the filter cake at 50-60 ℃ in vacuum until the weight is constant to obtain the 2-acrylamide-2-methylpropanesulfonic acid grafted cellulose acetate phthalate;
3) preparation of cellulose/hectorite hybrid composite material
Ultrasonically dispersing 2-acrylamide-2-methylpropanesulfonic acid grafted cellulose acetate phthalate in 80% V ethanol water solution, then adding hectorite nano material, ultrasonically treating for 1-2 days at 40-50 ℃, centrifuging, washing filter cakes with water, collecting the filter cakes, and drying the filter cakes at 45 ℃ to constant weight to obtain the cellulose/hectorite hybrid composite material.
Preferably, in step 3), the weight ratio of 2-acrylamide-2-methylpropanesulfonic acid grafted cellulose acetate phthalate: hectorite nano material is 1: 30-60; further preferably 1: 40.
Preferably, in step 1-B), lithium fluoride, magnesium hydroxide, and silica in molar ratios of 1:4: 8; the silica sol is a dispersion liquid of nano silica particles in water, and the weight percentage of silica in the dispersion liquid is 20%.
According to another aspect of the invention, the invention provides the use of a cellulose/hectorite hybrid composite material for the adsorptive purification of organic wastewater.
Preferably, the organic wastewater is phenol-containing wastewater, and the phenol-containing wastewater is one or a mixture of two or more of phenol wastewater, p-nitrophenol wastewater, p-chlorophenol wastewater and p-aminophenol, and is more preferably p-nitrophenol or p-aminophenol.
The invention has the following beneficial effects:
1) the invention takes grafted modified cellulose and hectorite as raw materials to prepare a novel cellulose/hectorite hybrid composite material;
2) the cellulose/hectorite hybrid composite material prepared by the invention can be used for adsorbing and purifying organic wastewater, especially phenolic substances in the wastewater;
3) the cellulose/hectorite hybrid composite material prepared by the method has high removal rate and adsorption capacity on phenolic wastewater, and particularly when cellulose acetate phthalate is used as a raw material, the removal rate of the phenolic wastewater is higher than that of the hybrid composite material prepared by the traditional cellulose;
4) the invention adds the ultrasonic process in the toluene solution of oleic acid when preparing hectorite, overcomes the defect that the hectorite nano material is easy to agglomerate;
5) because the hectorite can be uniformly dispersed in the water phase, the hectorite and the cellulose are hybridized and compounded, so that the prepared composite material can be fully dispersed in the water;
6) the hectorite and the cellulose acetate phthalate grafted by the 2-acrylamide-2-methylpropanesulfonic acid have a certain synergistic effect in the aspect of organic wastewater purification.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the description is intended to be exemplary only, and is not intended to limit the scope of the present invention.
Raw materials: cellulose acetate phthalate available from sigma aldrich trade ltd with a product designation of 22192 and a molecular weight of 2534.12 g/mol; coconut shell activated carbon (from Chinese medicine chemical reagent, product number 10006755, particle size 200 mesh); the rest raw materials are all conventional raw materials sold in the market.
In order to simulate the removal effect of the phenol-containing organic wastewater, a phenol-containing aqueous solution is prepared by the following method:
taking phenol-containing substance in an Erlenmeyer flask, adding 0.1mol/L H2SO4Or adjusting the pH value of the solution by 0.1mol/L NaOH aqueous solution, adding a certain amount of adsorbent, placing the conical flask into a 40 ℃ constant-temperature water bath oscillator, controlling the temperature at the rotating speed of 200r/min, stirring for 12h, filtering, and measuring the concentration of the phenol-containing substance by adopting an HPLC external standard method.
First, the adsorption quantity Q of the phenol-containing substancem(mg/g) see formula (1):
in the formula, C0And CtThe concentrations of phenol-containing substances in the solution at the initial stage and the adsorption equilibrium stage are mg/L respectively; v is the volume of the solution, L; m is the adsorbent amount, g. The test method refers to the measurement method specified in the national standard GB/T7702.8-2008.
Secondly, a detection method of the removal rate R of the phenol-containing substances comprises the following steps:
the removal rate R (%) of the phenol-containing substance in the aqueous solution was calculated by the formula (2):
in the formula, C0And C is the mass concentration of phenol in the initial filtrate and the filtrate, mg/L respectively.
Example 1
1) Preparing a hectorite nano material:
1-A) dissolving 100mmol of lithium fluoride in 200ml of water, then adding 400mmol of magnesium hydroxide, and stirring for 2-3h at 40-50 ℃ to obtain a first mixed solution;
1-B) dropping the first mixture into a silica sol (20% by weight SiO)2An aqueous dispersion of (A), SiO in the aqueous dispersion2The molar weight of the hectorite is 800mmol), stirring the mixture into a uniform mixture at the temperature of between 35 and 40 ℃, and then heating the mixture for reflux reaction for 16 to 18 hours to obtain hectorite dispersion liquid;
1-C) cooling the hectorite dispersion liquid to room temperature, centrifuging, collecting filter cakes, placing the filter cakes in a toluene solution of 0.5% V oleic acid, performing ultrasonic dispersion at the temperature of 80-90 ℃ for 1-2 days, cooling, centrifuging, collecting the filter cakes, heating to 180 ℃ at the heating rate of 5 ℃/min in the air atmosphere, and finally performing heat preservation and drying for 5-6h to obtain the hectorite nano material (the hectorite nano material is abbreviated as NanoH);
2) preparation of 2-acrylamido-2-methylpropanesulfonic acid grafted cellulose acetate phthalate:
2-A) preparing 100g of cellulose acetate phthalate into 6 wt% aqueous dispersion by using deionized water, and then adjusting the pH of the system to 2.0 by using hydrochloric acid to obtain cellulose acidic solution;
2-B) adding 0.5g of initiator ammonium ceric nitrate into the cellulose acidic solution, stirring and dissolving, heating to 50-60 ℃, adding 360mmol of 2-acrylamide-2-methylpropanesulfonic acid under nitrogen atmosphere, keeping the temperature and stirring for 1-2h to obtain 2-acrylamide-2-methylpropanesulfonic acid grafted cellulose acetate phthalate dispersion liquid;
2-C) centrifuging the 2-acrylamide-2-methylpropanesulfonic acid grafted cellulose acetate phthalate dispersion, washing a filter cake with water until the filtrate becomes neutral, collecting the filter cake, and drying the filter cake at 50-60 ℃ in vacuum until the weight is constant to obtain the 2-acrylamide-2-methylpropanesulfonic acid grafted cellulose acetate phthalate (the 2-acrylamide-2-methylpropanesulfonic acid grafted cellulose acetate phthalate is abbreviated as AC);
3) preparation of cellulose/hectorite hybrid composite material
Ultrasonically dispersing 1.0g of 2-acrylamide-2-methylpropanesulfonic acid grafted cellulose acetate phthalate in 200ml of 80% V ethanol aqueous solution, then adding 40.0g of hectorite nano material, ultrasonically treating the mixture at 40-50 ℃ for 2 days, centrifuging the mixture, washing a filter cake with water, collecting the filter cake, and drying the filter cake at 45 ℃ to constant weight to obtain the cellulose/hectorite hybrid composite material (the cellulose/hectorite hybrid composite material is abbreviated as AC/H).
Example 1-A
The cellulose acetate phthalate in example 1 was replaced with cellulose acetate by a one-way variable method, that is, cellulose acetate phthalate was replaced with equal weight of cellulose acetate as compared with example 1, and the rest was completely identical to the preparation method of example 1. The cellulose/hectorite hybrid composite material prepared is defined as C/H.
Example 2
For hectorite nanomaterial (NanoH) prepared in example 1, cellulose acetate phthalate (AC) grafted with 2-acrylamide-2-methylpropanesulfonic acid, cellulose/hectorite hybrid composite (AC/H), and C/H, the removal rate R of phenol (initial concentration of phenol C) of the adsorbent was measured at different pH values050mg/L and the amount of adsorbent added was 40mg/L), the results are shown in Table 1The following steps:
TABLE 1 removal of phenol at pH R with different adsorbents
Note: "-" represents no test; from front. environ. Sci. eng.2013,7(2): 158-165, removal of phenol by powdered activated carbon adsorption reported that coconut shell activated carbon has maximum adsorption activity at pH 9.0, so no test was performed at other pH conditions.
The results show that the cellulose/hectorite hybrid composite material (AC/H) prepared by the invention has stronger adsorption and purification effects on phenol, hectorite and 2-acrylamide-2-methylpropanesulfonic acid grafted cellulose acetate phthalate have certain synergistic effect, and the adsorption effect on phenol is far higher than that of coconut shell activated carbon.
Example 3
The removal rate R (initial concentration C of phenol-containing substance) of different phenol-containing substances was measured at different pH values using the cellulose/hectorite hybrid composite material (AC/H) prepared in example 1 as an adsorbent050mg/L and the amount of adsorbent added was 40mg/L), the results are shown in Table 2:
TABLE 2 removal rate R of different phenol-containing substances at different pH values
The test results show that the cellulose/hectorite hybrid composite material (AC/H) prepared by the invention has excellent adsorption removal effect on most phenol-containing substances, especially p-nitrophenol and p-aminophenol which have excellent adsorption performance in a wider pH range, and is convenient for actual industrial treatment.
Example 4
The cellulose/hectorite hybrid composite material (AC/H) prepared in example 1 was used as an adsorbent, and the adsorption amount Q corresponding to each phenol-containing substance was measured at the optimum adsorption pH of the phenol-containing substancem(of phenol-containing substances)Initial concentration C050mg/L), the results are shown in Table 3:
TABLE 3 adsorption amounts Q of different phenolic wastewatersm
| Phenol-containing substance | Phenol and its preparation | P-nitrophenol | P-chlorophenol | P-aminophenol | Catechol as one of the most important of the chemical substances in the chemical industry |
| 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 results show that the adsorption capacity Q of the cellulose/hectorite hybrid composite material (AC/H) prepared by the invention to different phenol-containing substancesmIn contrast, with p-nitrobenzeneThe phenol has the largest adsorption quantity and is far superior to the traditional wood activated carbon.
Although the embodiments of the present invention have been described in detail, it should be understood that various changes, substitutions, and alterations can be made hereto without departing from the spirit and scope of the invention.
Claims (7)
1. A preparation method of a cellulose/hectorite hybrid composite material is characterized by comprising the following steps: the cellulose/hectorite hybrid composite material is formed by carrying out ultrasonic hybridization on 2-acrylamide-2-methylpropanesulfonic acid grafted cellulose acetate phthalate and hectorite in an ethanol water solution; the method specifically comprises the following steps:
1) preparing a hectorite nano material:
1-A) adding magnesium hydroxide into a lithium fluoride aqueous solution, and stirring for 2-3h at 40-50 ℃ to obtain a first mixed solution;
1-B) dropwise adding the first mixed solution into silica sol, stirring at 35-40 ℃ to obtain a uniform mixture, and then heating for reflux reaction for 16-18h to obtain a hectorite dispersion solution;
1-C) cooling the hectorite dispersion liquid to room temperature, centrifuging, collecting filter cakes, placing the filter cakes in a toluene solution of 0.5% V oleic acid, performing ultrasonic dispersion for 1-2 days at the temperature of 80-90 ℃, cooling, centrifuging, collecting the filter cakes, heating to 180 ℃ at the heating rate of 5 ℃/min in the air atmosphere, and finally performing heat preservation and drying for 5-6h to obtain the hectorite nano material;
2) preparation of 2-acrylamido-2-methylpropanesulfonic acid grafted cellulose acetate phthalate:
2-A) preparing 100g of cellulose acetate phthalate into 5-8 wt% of aqueous dispersion by using deionized water, and then adjusting the pH of the system to 2.0 by using hydrochloric acid to obtain cellulose acidic solution;
2-B) adding 0.5g of initiator ammonium ceric nitrate into the cellulose acidic solution, stirring and dissolving, heating to 50-60 ℃, adding 300-400mmol of 2-acrylamide-2-methylpropanesulfonic acid under the nitrogen atmosphere, keeping the temperature and stirring for 1-2h to obtain 2-acrylamide-2-methylpropanesulfonic acid grafted cellulose acetate phthalate dispersion liquid;
2-C) centrifuging the 2-acrylamide-2-methylpropanesulfonic acid grafted cellulose acetate phthalate dispersion, washing a filter cake with water until the filtrate becomes neutral, collecting the filter cake, and drying the filter cake at 50-60 ℃ in vacuum until the weight is constant to obtain the 2-acrylamide-2-methylpropanesulfonic acid grafted cellulose acetate phthalate;
3) preparation of cellulose/hectorite hybrid composite material:
ultrasonically dispersing 2-acrylamide-2-methylpropanesulfonic acid grafted cellulose acetate phthalate in 80% V ethanol water solution, then adding hectorite nano material, ultrasonically treating for 1-2 days at 40-50 ℃, centrifuging, washing filter cakes with water, collecting the filter cakes, and drying the filter cakes at 45 ℃ to constant weight to obtain the cellulose/hectorite hybrid composite material.
2. The method of claim 1, wherein: in the step 3), the weight ratio of the 2-acrylamide-2-methylpropanesulfonic acid grafted cellulose acetate phthalate: hectorite nanomaterial =1: 30-60.
3. The method of claim 1, wherein: in the step 1-B), lithium fluoride, magnesium hydroxide and silicon dioxide =1:4:8 in terms of molar ratio; the silica sol is a dispersion liquid of nano silica particles in water, and the weight percentage of silica in the dispersion liquid is 20%.
4. Use of a cellulose/hectorite hybrid composite material obtained by the preparation method according to any one of claims 1 to 3, characterized in that: used for adsorbing and purifying organic wastewater.
5. Use according to claim 4, characterized in that: the organic wastewater is phenol-containing wastewater.
6. Use according to claim 5, characterized in that: the phenol-containing wastewater is one or the mixture of more than two of phenol wastewater, p-nitrophenol wastewater, p-chlorophenol wastewater and p-aminophenol wastewater.
7. Use according to claim 6, characterized in that: the phenol-containing wastewater is p-nitrophenol wastewater or p-aminophenol wastewater.
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| CN102500339A (en) * | 2011-12-05 | 2012-06-20 | 福州大学 | Reductive spherical cellulose adsorbent containing sulfinyl and preparation method thereof |
| CN103497278A (en) * | 2013-10-16 | 2014-01-08 | 苏州大学 | Amphoteric cellulose material and application thereof |
| CN104126870A (en) * | 2014-07-18 | 2014-11-05 | 云南中烟工业有限责任公司 | Manufacturing method and application of anionic polymer modified cellulose acetate |
| CN105621523A (en) * | 2016-03-18 | 2016-06-01 | 沈阳化工大学 | Method for treating phenolic waste water through gel adsorbent |
| CN107555521A (en) * | 2017-10-27 | 2018-01-09 | 卢伟 | A kind of heavy metal-polluted water process multiporous biological matter microballoon and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102500339A (en) * | 2011-12-05 | 2012-06-20 | 福州大学 | Reductive spherical cellulose adsorbent containing sulfinyl and preparation method thereof |
| CN103497278A (en) * | 2013-10-16 | 2014-01-08 | 苏州大学 | Amphoteric cellulose material and application thereof |
| CN104126870A (en) * | 2014-07-18 | 2014-11-05 | 云南中烟工业有限责任公司 | Manufacturing method and application of anionic polymer modified cellulose acetate |
| CN105621523A (en) * | 2016-03-18 | 2016-06-01 | 沈阳化工大学 | Method for treating phenolic waste water through gel adsorbent |
| CN107555521A (en) * | 2017-10-27 | 2018-01-09 | 卢伟 | A kind of heavy metal-polluted water process multiporous biological matter microballoon and preparation method thereof |
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