CN101721978A - Adsorbent for polyaromatic hydrocarbon pollutant, preparation method and application thereof - Google Patents
Adsorbent for polyaromatic hydrocarbon pollutant, preparation method and application thereof Download PDFInfo
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- CN101721978A CN101721978A CN200910201394A CN200910201394A CN101721978A CN 101721978 A CN101721978 A CN 101721978A CN 200910201394 A CN200910201394 A CN 200910201394A CN 200910201394 A CN200910201394 A CN 200910201394A CN 101721978 A CN101721978 A CN 101721978A
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Abstract
The invention discloses a method for preparing an absorbent for a polyaromatic hydrocarbon pollutant. The method comprises the following step that: a biomass porous adsorption material and cationic surfactant are subjected to modification reaction, wherein a cationic surfactant comprises a quaternary ammonium cationic surfactant and a polymeric cationic surfactant, and is a cationic surfactant, of which the molecules carry C8-C24 alkyl, which can be dissolved in water, can generate ionization, and can remarkably affect wettability between solid and liquid. The invention also discloses the adsorbent for the polyaromatic hydrocarbon pollutant and application thereof. The adsorbent for the polyaromatic hydrocarbon pollutant can be used for polyaromatic hydrocarbon treatment of domestic sewage advanced treatment, and removal rate can be over 95 percent; and the preparation method has the advantages of wide raw material sources, low cost and simple process.
Description
Technical field
The present invention is specifically related to adsorbent of a kind of polyaromatic hydrocarbon pollutant and its production and application.
Background technology
Persistence organic pollutant such as polycyclic aromatic hydrocarbon (PAHs) are that the difficult natural degradation of a class has three compounds that cause effect.Majority has stronger toxicity, and its harm is wide, can exist lastingly in environment, belongs to preferential control pollutant.Persistence organic pollutant except that natural cause generates, mainly from the process of utilizing of the mankind's activity and the energy, as the burning of oil, coal etc., oil and petrochemicals production, the processes such as spill and leakage in offshore oil development and the transportation.
Polyaromatic hydrocarbon pollutant has than strong-hydrophobicity, and is difficult to by biodegradation, but under the condition that surfactant or a small amount of solvent exist, and can dissolve to be in the water, enters environment water with face of land runoff or sewage discharge.In a single day these organic pollutions enter in the natural environment by water body, easily attached in bed mud in river and the soil, and enrichment in vivo, its concentration can finally cause serious harm to organism by constantly accumulation and amplification of biological chain.Most of river of nationwide all has been subjected to the pollution of polycyclic aromatic hydrocarbon at present; the accumulation of polycyclic aromatic hydrocarbon in environment more and more seriously threatened human beings'health; therefore how to administer polycyclic aromatic hydrocarbons contaminated; to help people to protect environment, environment purification better, thus the human health of maintenance.
Present processing method to trade effluent has a variety of, as activated sludge process, and advanced oxidation processes, absorption method or the like.Activated sludge process is difficult to effectively remove the multiring aromatic hydrocarbon organic pollution as traditional method for treating water owing to be subjected to the restriction of microorganism.Though adopt advanced oxidation processes to degrade to these organic matters, it handles energy consumption height, reagent dosage is big, device is huge, complicated operation and easily form secondary pollution, and is not good to the multiring aromatic hydrocarbon removal effect of organic matter of the low concentration that exists in the water.
More be to adopt absorption method to handle polycyclic aromatic hydrocarbon in the water at present in the world, active carbon for example, organic clay, resin, sorbing materials such as peat, but material cost height such as active carbon, resin, and adsorb and be difficult to regeneration after saturated and handle; Peat is cheap, adsorb to can be used as fuel after saturated, but its absorption property is limited, and has the risk of humic acid stripping secondary pollution.Thereby how to develop that a kind of technology is simple, the new adsorbent of economical and efficient, and be applied to the problem that people pay close attention to that is treated as of polycyclic aromatic hydrocarbon in the water.
Summary of the invention
Technical problem to be solved by this invention is to be difficult to defective such as regeneration processing after saturated for the sorbing material cost height that overcomes the polycyclic aromatic hydrocarbon in the existing processing water, absorption, and adsorbent of a kind of polyaromatic hydrocarbon pollutant and its production and application is provided.The adsorbent of polyaromatic hydrocarbon pollutant of the present invention can be used for the processing of treatment of domestic sewage advanced polycyclic aromatic hydrocarbon, and clearance is higher than 95%; And in its preparation method, the raw material wide material sources, cheap, technology is simple.
The inventor is through discovering in a large number, when biomass porous sorbing material such as peat, after cationic surfactant such as CTAB modification, CTAB has increased the specific area of biomass porous sorbing material, increased the activity on its surface, enriched its surperficial functional group, made it have lipophile preferably, the adsorption capacity of lipophilicity substance has significantly been strengthened.
Therefore the present invention relates to a kind of preparation of adsorbent method of polyaromatic hydrocarbon pollutant, it comprises the following step: biomass porous sorbing material and cationic surfactant are carried out modified-reaction, get final product; Wherein, described cationic surfactant is to have C in the molecule
8～C
24Alkyl, can be water-soluble, ionization can take place, can influence the cationic surfactant of solid liquid interface wetability, it comprises quaternary ammonium salt and polymerizing cationically cationoid surfactant.The straight chained alkyl that described alkyl is preferable.When carbon number was identical, the dication surfactant was better than single cationic surfactant.
Wherein, described biomass porous sorbing material is meant and derives from (agricultural in the natural environment, forestry etc.) biological material, being characterized as material itself has than multiple aperture, and pore-size distribution is fit to be adsorbed with the material of organic pollutants, in preferable is peat, pine bark, wheat straw stalk, straw, wood chip, palm palm fibre skin, walnut shell, shredded coconut meat, cornstalk and the pine tree fallen leaves etc. one or more, preferred peat.
Among the present invention, described quaternary cationic surfactant is preferable is in softex kw (CTAB), cetyl pyridinium bromide and the TBAB one or more, preferred softex kw, what described polymerizing cationically cationoid surfactant was preferable is poly-epoxychloropropane dimethylamine (EPI-DMA) and/or methylacryoyloxyethyl dodecyl dimethyl ammonium bromide (DMDB).When described biomass porous sorbing material is peat, the preferred softex kw of described cationic surfactant (CTAB).
Among the present invention, what the mass ratio of described biomass porous sorbing material and cationic surfactant was preferable is 1: 0.1 to 1: 1.0; What the method for described modified-reaction was preferable reacts for soaking, be about to carry out modified-reaction in the solution (preferred aqueous solutions) that biomass porous sorbing material is immersed in cationic surfactant, what the temperature of soaking was preferable is 20～80 ℃, and what the time of immersion was preferable is 4～10 hours.When biomass porous sorbing material is a peat, when cationic surfactant is softex kw, the method of modified-reaction is for soaking reaction, preferred 20～40 ℃ of the temperature of immersion in the aqueous solution that the peat of particle diameter 20～200 purposes is immersed in softex kw; That the concentration of the aqueous solution of softex kw is preferable is 0.01～0.50mol/L.
Among the present invention, preferable after described modified-reaction finishes, with the biomass porous sorbing material washed with de-ionized water after the modification, oven dry gets final product then.What wherein, the temperature of oven dry was preferable is 80 ℃.
Among the present invention, the preparation of adsorbent method of described polyaromatic hydrocarbon pollutant is preferable also comprises the following step: before modified-reaction, biomass porous sorbing material water or alkali are cleaned.Wherein, the preferred peat of described biomass porous sorbing material improving pore-size distribution and specific area, and is removed humic acid wherein by clear water or alkali cleaning peat; What described biomass porous sorbing material was preferable uses for pulverizing the back, and what its particle diameter was preferable is 40～200 orders; The step of cleaning with alkali can be the conventional steps of biomass porous sorbing material such as this area basification peat, and is preferable for biomass porous sorbing material is soaked in alkali lye, stirring, filter, the biomass porous sorbing material that filter is done is extremely neutral with washed with de-ionized water, and oven dry gets final product.Wherein, what described alkali lye was preferable is the aqueous solution of NaOH or KOH, and that its concentration is preferable is 0.001-0.01mol/L, and what pH was preferable is 12; What the time of described immersion was preferable is 5-40 minute, preferred 15 minutes.
Among the present invention, when described biomass porous sorbing material was peat, the optimization procedure of the preparation of adsorbent method of described polyaromatic hydrocarbon pollutant was as follows:
The peat crushing screening is got sample between 40～200 orders, adding the pH value and be 12 NaOH stirs and soaks 15min, filter, filtrate is humic acid solution, to filter again the peat done with deionized water clean repeatedly to filtrate pH value be 7, with peat 90 ℃ of oven dry, the peat of getting a certain amount of oven dry is immersed at a certain temperature in the CTAB solution of 0.01～0.50mol/L and carries out modification, wherein the ratio of peat and CTAB is 1: 0.1～1: 1.0 (mass ratio), and soaking temperature is 30～80 ℃, and soak time is 4～8h, with the modified turf washed with de-ionized water, to the non-foam generation, 90 ℃ of oven dry get final product.
Among the preparation method of the present invention, above-mentioned each optimum condition can the conventional knowledge in this area be according to making up arbitrarily, promptly making each preferred embodiments of the present invention.
The invention further relates to the adsorbent of the polyaromatic hydrocarbon pollutant that above-mentioned preparation method makes.
Application in the polyaromatic hydrocarbon pollutant of the adsorbent that the invention still further relates to above-mentioned polyaromatic hydrocarbon pollutant in removing water.
Polyaromatic hydrocarbon pollutant shows lipophile mostly, with compare before the modification, the adsorbent lipophilic group of polyaromatic hydrocarbon pollutant of the present invention increases, lipophile significantly increases, polyaromatic hydrocarbon pollutant in the good adsorbed water of energy, water outlet is effective, is applicable to by polycyclic aromatic hydrocarbons contaminated micro-polluted water territory.
Except that specified otherwise, raw material that the present invention relates to and reagent are all commercially available to be got.
Positive progressive effect of the present invention is:
(1) among the preparation method of the present invention, the raw material wide material sources, cheap, technology is simple.
(2) adsorbent of polyaromatic hydrocarbon pollutant of the present invention can be used for the processing of treatment of domestic sewage advanced polycyclic aromatic hydrocarbon, and clearance can be higher than 95%.
(3) adsorbent of the preferred polyaromatic hydrocarbon pollutant of the present invention has not only overcome peat humic acid stripping when handling water pollutant, water body is caused secondary pollution problem, but also can reclaim humic acid, with the humic acid that reclaims as industrial water conditioning agent or feed addictive raw material.
Description of drawings
The sem photograph of the adsorbent of the polyaromatic hydrocarbon pollutant that Fig. 1 makes for embodiment 1.
Fig. 2 is the time (abscissa) of sample B in n-hexane second and pressure differential deltap P (ordinate) millibar graph of a relation before the modification among the embodiment 1.
Fig. 3 is the time (second, abscissa) of sample C in n-hexane and the graph of a relation of pressure differential deltap P (millibar, ordinate) after the modification that makes among the embodiment 1.
The specific embodiment
Further specify the present invention with embodiment below, but the present invention is not limited.
Below among each embodiment, raw material peat is that Dunhua City, Jilin Province lucky peat development Co., Ltd produces; Rice straw is from the paddy rice of Shexian County, Huangshan, Anhui Province in September, 2008 harvesting; Pine bark is taken from the crust of the 5 years living Korean pines in Chifeng City, the Inner Mongol.
Embodiment 1
Natural peat was pulverized the 100-200 mesh sieve, take by weighing in the 1250ml NaOH solution of the pH=12 that the 10g natural peat joins, 500r/m stirs 20min, suction filtration, use washed with de-ionized water until 7,80 ℃ of rinse water pH ≈ oven dry 10h repeatedly, obtain the peat (alkali cleaning peat B) after the alkali cleaning.Take by weighing alkali cleaning peat 5g again, according to peat: CTAB: the ratio of water=1: 1: 250 (mass ratio) is carried out modification, 55 ℃ of water-bath vibration 6h, rotating speed 150r/m, with the solution suction filtration, produce after reaction is finished, take out at 80 ℃ and dry 10h down with washed with de-ionized water to non-foam, grinding sieves makes alkali cleaning modified turf (modified turf C), gets final product.The modified turf that above-mentioned steps makes is made the SEM scanning electron microscope analysis, and the photo that obtains is seen Figure of description 1.
Embodiment 2
Natural peat was pulverized the 100-200 mesh sieve, take by weighing among the 1250ml, NaOH solution of the pH=12 that the 10g natural peat joins, 500r/m stirs 20min, suction filtration, use washed with de-ionized water until 7,80 ℃ of rinse water pH ≈ oven dry 10h repeatedly, obtain the peat after the alkali cleaning.Take by weighing alkali cleaning peat 5g again, according to peat: CTAB: the ratio of water=1: 1: 250 (mass ratio) is carried out modification, 40 ℃ of water-bath vibration 6h, rotating speed 150r/m, with the solution suction filtration, produce after reaction is finished, take out at 80 ℃ and dry 10h down with washed with de-ionized water to non-foam, grinding sieves makes the alkali cleaning modified turf, gets final product.Alkali cleaning peat that above-mentioned steps is worth and modified turf at room temperature (25 ℃) to 50ml, the luxuriant and rich with fragrance solution of 1mg/L carries out static adsorption test, behind the 12h, the maximal absorptive capacity of natural peat is 0.75mg/g, the maximal absorptive capacity of alkali cleaning peat is 0.83mg/g.The maximal absorptive capacity of modified turf is 1.65mg/g, compares natural peat the adsorbance of phenanthrene has been improved 120%.
Embodiment 3
100 mesh sieves were pulverized in natural straw stalk oven dry, taken by weighing 20g natural straw powder and join among the 1250ml, NaOH solution of pH=12,500r/m stirs 30min, suction filtration, use washed with de-ionized water until 7,80 ℃ of rinse water pH ≈ oven dry 10h repeatedly, obtain the straw after the alkali cleaning.Take by weighing alkali cleaning straw 10g again, according to straw: TBAB (TBAB): the ratio of water=1: 0.5: 250 (mass ratio) is carried out modification, 80 ℃ of water-bath vibration 6h, rotating speed 150r/m, with the solution suction filtration, produce after reaction is finished, take out at 80 ℃ and dry 10h down with washed with de-ionized water to non-foam, grinding sieves makes alkali cleaning TBAB modification straw, gets final product.Alkali cleaning straw that above-mentioned steps is worth and modification straw at room temperature (25 ℃) to 100ml, the luxuriant and rich with fragrance solution of 1mg/L carries out static adsorption test, behind the 12h, the adsorbance of natural straw is 0.49mg/g, the adsorbance of alkali cleaning straw is 0.61mg/g.The adsorbance of modification straw is 0.70mg/g.
Embodiment 4
With the oven dry of Korean pine bark, pulverized 40 mesh sieve powderings, take by weighing 10g and use washed with de-ionized water repeatedly until non-foam and 7,105 ℃ of oven dry of rinse water pH ≈ 10h, obtain washing the pine bark powder.Take by weighing the washing pine bark powder 5g of oven dry, according to raw material: the cetyl pyridinium bromide: the ratio of water=1: 0.5: 250 (mass ratio) is carried out modification, 30 ℃ of water-bath vibration 10h, rotating speed 150r/m, with the solution suction filtration, produce after reaction is finished, take out at 105 ℃ and dry 10h down with washed with de-ionized water to non-foam, grinding sieves makes the modification bark, gets final product.Washing bark that above-mentioned steps is made and modification bark under 30 ℃ of conditions to 50ml, the luxuriant and rich with fragrance solution of 1mg/L carries out static adsorption test, behind the 12h, the maximal absorptive capacity of washing bark is 0.80mg/g, the maximal absorptive capacity of modification bark is 1.33mg/g, compares the washing bark adsorbance of phenanthrene is improved a lot.
Effect embodiment 1
Taking by weighing natural peat 0.3g adding 500ml concentration is containing in the naphthalene waste water of 1.53mg/L, and adsorption treatment is after 1 hour, and going out water concentration is 1.19mg/L, and clearance is 22.2%; Taking by weighing modified turf 0.3g (through alkali cleaning, CTAB modification, preparation condition such as embodiment 1) adding 500ml concentration is containing in the naphthalene waste water of 1.53mg/L, adsorbs after 1 hour, and going out water concentration is 0.81mg/L, and clearance is 47.0%, has improved 24.8%.
Effect embodiment 2
Adopt the 0.6g natural peat, the industrial wastewater that is 0.96mg/L to the luxuriant and rich with fragrance concentration of 1L carries out adsorption treatment, and adsorption equilibrium is after 1.5 hours, and the Sino-Philippines concentration of waste water is 0.116mg/L, and clearance is 87.9%; Adopt 0.6g CTAB modified turf (through alkali cleaning and CTAB modification, preparation condition is with embodiment 1), the industrial wastewater that is 0.96mg/L to the luxuriant and rich with fragrance concentration of 1L carries out adsorption treatment, and adsorption equilibrium is after 1.5 hours, the Sino-Philippines concentration of waste water is reduced to 0.042mg/L, and clearance is 95.6%.
Effect embodiment 3
Adopt the 0.6g natural peat, the industrial wastewater that is 0.96mg/L to the luxuriant and rich with fragrance concentration of 1L carries out adsorption treatment, and adsorption equilibrium is after 4 hours, and the Sino-Philippines concentration of waste water is 0.10mg/L, and clearance is 89.6%; (preparation method of this alkali cleaning CTAB modified turf is as follows: the peat after the preparation alkali cleaning earlier to adopt 0.6g alkali cleaning CTAB modified turf, this step is with described in the embodiment 1, get alkali cleaning peat then, according to peat: CTAB: water=1: 0.1: 200 (mass ratio) ratio is carried out modification, 4h is soaked in 30 ℃ of water-bath vibrations, rotating speed 150r/m, the reaction finish after with the solution suction filtration, produce with washed with de-ionized water to non-foam, taking-up is dried 12h down at 80 ℃, ground 40 mesh sieves and obtained alkali cleaning CTAB modified turf), the industrial wastewater that is 0.96mg/L to the luxuriant and rich with fragrance concentration of 1L carries out adsorption treatment, after the adsorption equilibrium 4 hours, the Sino-Philippines concentration of waste water is reduced to 0.01mg/L, and clearance is 99.0%.
Effect embodiment 4
Adopt the 0.6g natural peat, the industrial wastewater that is 1.03mg/L to the luxuriant and rich with fragrance concentration of 200mL carries out adsorption treatment, and adsorption equilibrium is after 2 hours, and the Sino-Philippines concentration of waste water is 0.37mg/L, and clearance is 64.1%; (preparation condition of this modified turf is: take by weighing among the 1250ml, NaOH solution of the pH=12 that the unmodified peat of 10g joins to adopt 0.6g alkali cleaning poly-epoxychloropropane dimethylamine (EPI-DMA) modified turf, 500r/m stirs 30min, suction filtration, use washed with de-ionized water until rinse water pH ≈ 7 repeatedly, 80 ℃ of oven dry 10h obtain alkali cleaning peat.Take by weighing alkali cleaning peat 5g, in peat: EPI-DMA: water=1: 0.5: 200 (mass ratio) ratio is carried out modification, 6h is soaked in 50 ℃ of water-bath vibrations, rotating speed 200r/m, the reaction finish after with the solution suction filtration, produce with washed with de-ionized water to non-foam, taking-up is dried 12h down at 80 ℃, ground 40 mesh sieves and obtained alkali cleaning EPI-DMA modified turf), the industrial wastewater that is 1.03mg/L to the luxuriant and rich with fragrance concentration of 200mL carries out adsorption treatment, and adsorption equilibrium is after 2 hours, and the Sino-Philippines concentration of waste water is reduced to 0.12mg/L, clearance is 88.3%, and is higher by 24.2% than unmodified peat clearance.
Effect embodiment 5
Test before the modification sample B and the time of sample C in n-hexane and the relation of pressure reduction after the modification, the results are shown in Figure 2 and Fig. 3.Wherein, sample B and C are alkali cleaning peat B and the modified turf C among the embodiment 1.
Experiment conclusion: through after the modification, sample is greatly improved to the wetability (lipophile) of n-hexane, being embodied in wetting pressure reduction significantly increases, and by the calculating feeler that connects: if assumes samples C is to contact angle θ=0 of n-hexane, the sample B feeler that connects is 61.
Wherein, the wetability measuring method is as follows: JF99A powder contact angle instrument (Shanghai Zhongchen digital technology equipment Co., Ltd's production); Condition determination: the heavy B:0.4067g of sample; C:0.4080g; Bake out temperature: 110 ℃ (2 hours); Measure temperature: 25 ± 0.5 ℃; Wetting agent: n-hexane (Y=18.4mN/m; η=0.307mPaS).
Claims (12)
1. the preparation of adsorbent method of a polyaromatic hydrocarbon pollutant is characterized in that comprising the following step: biomass porous sorbing material and cationic surfactant are carried out modified-reaction, get final product; Wherein said cationic surfactant comprises quaternary ammonium salt and polymerizing cationically cationoid surfactant, and it has C in the molecule
8～C
24Alkyl, can be water-soluble, ionization can take place, can appreciable impact solid-liquid body between the cationic surfactant of wetability.
2. preparation method as claimed in claim 1 is characterized in that: described biomass porous sorbing material is one or more of peat, pine bark, wheat straw stalk, straw, wood chip, palm palm fibre skin, walnut shell, shredded coconut meat, cornstalk and pine tree fallen leaves.
3. preparation method as claimed in claim 1 is characterized in that: described alkyl is a straight chained alkyl.
4. preparation method as claimed in claim 1 is characterized in that: described quaternary cationic surfactant is one or more in softex kw, cetyl pyridinium bromide and the TBAB; Described polymerizing cationically cationoid surfactant is poly-epoxychloropropane dimethylamine and/or methylacryoyloxyethyl dodecyl dimethyl ammonium bromide.
5. preparation method as claimed in claim 1 is characterized in that: when described biomass porous sorbing material was peat, described cationic surfactant was a softex kw.
6. preparation method as claimed in claim 1 is characterized in that: the mass ratio of described biomass porous sorbing material and cationic surfactant is 1: 0.1 to 1: 1.0; The method of described modified-reaction is for carrying out modified-reaction in the solution that biomass porous sorbing material is immersed in cationic surfactant.
7. preparation method as claimed in claim 6 is characterized in that: the temperature of described immersion is 20～80 ℃, and the time of immersion is 4～10 hours.
8. preparation method as claimed in claim 6, it is characterized in that: when biomass porous sorbing material is a peat, when cationic surfactant is softex kw, the method of modified-reaction is for soaking reaction in the aqueous solution that the peat of particle diameter 20～200 purposes is immersed in softex kw, and the temperature of immersion is 20～40 ℃; The concentration of the aqueous solution of softex kw is 0.01～0.50mol/L.
9. preparation method as claimed in claim 1 is characterized in that: after described modified-reaction finished, with the biomass porous sorbing material washed with de-ionized water after the modification, oven dry got final product then.
10. preparation method as claimed in claim 1 is characterized in that: the preparation of adsorbent method of described polyaromatic hydrocarbon pollutant also comprises the following step: before modified-reaction, biomass porous sorbing material water or alkali are cleaned.
11. the adsorbent of the polyaromatic hydrocarbon pollutant that makes as each described preparation method of claim 1～10.
12. the application in the polyaromatic hydrocarbon pollutant of the adsorbent of polyaromatic hydrocarbon pollutant as claimed in claim 11 in removing water.
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