CN102658100B - Preparation method of polyacrylic acid-humic acid-rectorite composite adsorbing agent - Google Patents
Preparation method of polyacrylic acid-humic acid-rectorite composite adsorbing agent Download PDFInfo
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Abstract
The invention discloses a preparation method of a polyacrylic acid-humic acid-rectorite composite adsorbing agent, which adopts organic quaternary ammonium salt and rectorite to generate a cation exchange reaction to form organic rectorite, then enables the crylic acid to conduct in-situ polymerization on a nanometer interlayer of the organic rectorite to form an intercalation polymer/ clay composite material, simultaneously loads the humic acid, and prepares the polyacrylic acid-humic acid-rectorite composite adsorbing agent. The preparation method takes full advantage of the rectorite and the humic acid on excellent adsorbability of polycyclic aromatic hydrocarbon and high-efficient adsorbability of polyacrylic acid on heavy metal, enables the adsorbing agent to simultaneously adsorbing the heavy metal and the polycyclic aromatic hydrocarbon, and simultaneously expresses the superiority of the polyacrylic resin on rate of adsorption. The adsorbing agent is high in adsorption efficiency of the heavy metal and the polycyclic aromatic hydrocarbon, and rapid in adsorption speed of the heavy metal and the polycyclic aromatic hydrocarbon.
Description
Technical field
The invention belongs to material for water treatment technical field, relate to specifically a kind of preparation technology of organic/inorganic compound adsorbent.
Background technology
Heavy metal and polycyclic aromatic hydrocarbon are the persistent pollutants of two quasi-representatives in environment, are therefore the study hotspots of field of environment engineering to heavy metal and polycyclic aromatic hydrocarbons contaminated improvement.Heavy metal and polycyclic aromatic hydrocarbons contaminated improvement adopt absorption method conventionally, and the adsorbent of industrial use is mainly active carbon and preparation, but this two classes adsorbent is expensive, and regeneration difficulty, has limited its application to a certain extent.In recent years, the study hotspot of field of waste water treatment to the exploitation of cheap and the adsorbent that adsorption efficiency is high always, but, research and development to sorbing material at present, only, for single heavy metal or single polycyclic aromatic hydrocarbon, not yet someone develops the adsorbent of energy while efficient adsorption heavy metal and polycyclic aromatic hydrocarbon.In fact, heavy metal and polycyclic aromatic hydrocarbon often simultaneously or successively in entered environment, form heavy metal and polycyclic aromatic hydrocarbon composite pollution.As contained a large amount of heavy metals and polycyclic aromatic hydrocarbon in the creasote of timber preservative factory use, they conventionally can be detected in environment simultaneously.At present, China's surface water body is generally subject to the combined pollution of heavy metal and polycyclic aromatic hydrocarbon, and as Taihu Lake basin, South Lake, Changchun etc., wherein, all detect at South Lake Heavy Metals in Waters lead, cadmium, copper, zinc and polycyclic aromatic hydrocarbon fluorenes, phenanthrene, anthracene, pyrene.Can there is chemical interaction in the heavy metal in environment and polycyclic aromatic hydrocarbon, as formed heavy metal organic complex etc., these complex compounds, with respect to Single Pollution thing, will produce more complex environment effect, cause more serious environmental pollution.Therefore, the improvement of heavy metal-polycyclic aromatic hydrocarbon composite pollution will more and more receive people's concern, and the sorbing material of developing a kind of heavy-metal ion removal simultaneously and multiring aromatic hydrocarbon substance is significant for the reparation of heavy metal and polycyclic aromatic hydrocarbon composite pollution water body.
In recent years, along with composite organic-inorganic material going deep in the application study in each field, it is that raw material is prepared polyalcohol/clay soil composite adsorbing material that existing researcher adopts organic matter and inorganic clay, due to the introducing of inorganic component, has reduced the preparation cost of adsorbent.But the polyalcohol/clay soil composite adsorbing material of having developed, is mainly used in adsorbing heavy metal ion and the dye of positive ion etc. that hydrophily is strong, can not adsorb hydrophobic organic pollutant, as polycyclic aromatic hydrocarbon etc.
Summary of the invention
Goal of the invention: for the problem and shortage of above-mentioned existing existence, the object of this invention is to provide the preparation method of a kind of polyacrylic acid-humic acid-rectorite compound adsorbent, this adsorbent has excellent absorption property to heavy metal in water and polyaromatic hydrocarbon pollutant simultaneously, overcome existing polyalcohol/clay soil composite adsorbing material only for adsorbing heavy metal ion and the dye of positive ion etc. that hydrophily is strong, can not adsorb the drawback of hydrophobic organic pollutant, for the improvement of heavy metal and polycyclic aromatic hydrocarbon composite pollution provides new material.
Technical scheme: for achieving the above object, the present invention by the following technical solutions: the preparation method of a kind of polyacrylic acid-humic acid-rectorite compound adsorbent, is characterized in that comprising the following steps:
(1) preparation of organic rectorite: 5 ~ 15 parts of rectorites are added in 50 ~ 150 parts of water, stir, be mixed with rectorite water slurry, add 0.5 ~ 2 part of quaternary ammonium salt, regulate pH value to 5.5 ~ 6.5, and under 60 ~ 70 ℃ of water-baths stirring reaction 18 ~ 24h, then wash by deionized water, until the halide ion of noresidue, and through super-dry, be ground to 180 ~ 240 orders, obtain organic rectorite;
(2) preparation of acrylic acid aqueous solution: take 1.0 ~ 1.5 parts of acrylic acid, add in 20 ~ 30 parts of deionized waters, dissolve; Then add 0.3 ~ 0.8 part of NaOH, stirring reaction 10 ~ 20min;
(3) polymerisation: the acrylic acid aqueous solution that step (2) is obtained is transferred in reaction vessel, and under the protection of inert gas, add 2 ~ 3 parts of organic rectorites and 0.1 ~ 0.5 part of humic acid, fully stir 10min, slowly add 0.002 ~ 0.01 part of crosslinking agent and 0.01 ~ 0.05 part of initator, temperature is risen to 40 ~ 50 ℃, and prepolymerization 25 ~ 40min, is then warming up to 60 ~ 80 ℃ of reaction 2 ~ 3h;
(4) product of (3) step is fully washed with ethanol, then dry at 70 ~ 85 ℃, be ground to 180 ~ 240 orders, obtain polyacrylic acid-humic acid-rectorite compound adsorbent;
In above-mentioned preparation process, the umber of each material is mass fraction.
As preferably, described quaternary ammonium salt is any one in softex kw, cetalkonium chloride, TTAB, myristyl dimethyl benzyl ammonium chloride or dodecyl benzyl dimethyl ammonium chloride.
As preferably, described crosslinking agent is N, N '-methylene-bisacrylamide; Described initator is potassium peroxydisulfate.
Beneficial effect: compared with prior art, the present invention has the following advantages: (1) the present invention makes full use of rectorite and good adsorption capacity and the polyacrylic acid efficient adsorption ability to heavy metal of humic acid to polycyclic aromatic hydrocarbon, make adsorbent Adsorption of Heavy Metals and the polycyclic aromatic hydrocarbon simultaneously of invention, simultaneously, brought into play the fast advantage of adsorption rate of polyacrylic resin, the adsorption efficiency of this ABSORBENTS ABSORPTION metal and polycyclic aromatic hydrocarbon is high, adsorption rate is fast; (2) the present invention makes acrylic acid polymerization between the nanometer layer of rectorite, make the increase of rectorite interlamellar spacing, hydrophobicity strengthen, increase new adsorption site, the adsorbent of preparation is improved the adsorption capacity of hydrophobic organic compound, add the absorption of humic acid to polycyclic aromatic hydrocarbon, make this adsorbent in guaranteeing the efficient adsorption of heavy metal, polycyclic aromatic hydrocarbon is also had to good adsorption effect, and having overcome similar adsorbent can only Adsorption of Heavy Metals, can not adsorb the drawback of hydrophobic contaminant; (3) heavy metal class with polyaromatic hydrocarbon pollutant on this adsorbent adsorption mechanism different with adsorption site position, there is not competitive Adsorption, can use this adsorbent efficient removal heavy metal and polycyclic aromatic hydrocarbon from water simultaneously, for contain the wastewater treatment of heavy metal and polycyclic aromatic hydrocarbon and be subject to polycyclic aromatic hydrocarbon and the reparation of heavy-metal composite pollution water body simultaneously; (4) the present invention adopts the in-situ inserted polymerization of the aqueous solution to prepare adsorbent, not with an organic solvent, and non-secondary pollution.
The specific embodiment
Below in conjunction with specific embodiment, further illustrate the present invention, should understand these embodiment is only not used in and limits the scope of the invention for the present invention is described, after having read the present invention, those skilled in the art all fall within the application's claims limited range to the modification of the various equivalent form of values of the present invention.
Because polyacrylic acid resinoid has higher adsorption capacity to the heavy metal in water, and adsorption rate is fast, rectorite mineral and humic acid all have good adsorption capacity to heavy metal and polycyclic aromatic hydrocarbon, by composite to acrylic acid, humic acid and rectorite synthetic compound adsorbent, can make full use of rectorite and humic acid good adsorption capacity and the efficient adsorption ability of polyacrylic acid to heavy metal to polycyclic aromatic hydrocarbon, the fast advantage of performance polyacrylic resin adsorption rate, quick adsorption is removed heavy metal and the polycyclic aromatic hydrocarbon in water simultaneously.Adopt organic quaternary ammonium salt and rectorite generation cation exchange reaction to form organic rectorite, then make acrylic acid in-situ polymerization between the nanometer layer of organic rectorite, form intercal type polyalcohol/clay soil composite, humic acid in load simultaneously, makes polyacrylic acid-humic acid-rectorite compound adsorbent.
Embodiment 1:
Take 10 parts of rectorites and add in 100 parts of water and be mixed with rectorite water slurry, then add 1.0 parts of softex kws, regulate pH value to 6.5, stirring reaction 24h under 70 ℃ of water-baths, product washs by a large amount of deionized waters, until noresidue Br
-till, dry, be ground to 200 orders, obtain organic rectorite.Take 1.2 parts of acrylic acid, add in 25 parts of deionized waters, dissolve.Then under ice-water bath condition, add 0.5 part of NaOH, stirring reaction 10min.Aforesaid propylene aqueous acid is transferred in four-hole boiling flask, at N
2under protection, add 2.6 parts of organic rectorites and 0.2 part of humic acid, fully stir 10min; then slowly add 0.005 part of crosslinking agent N, N '-methylene-bisacrylamide and 0.03 part of initiator potassium persulfate, by warming-in-water to 40 ℃; prepolymerization 30min, is then warming up to 70 ℃ of reaction 3h.After reaction finishes, product is fully washed with ethanol, dry at 70 ℃, be ground to 200 orders, obtain polyacrylic acid-humic acid-rectorite compound adsorbent.
The Pb that configuration 1.0L concentration is 50mg/L
2+solution, adds the polyacrylic acid-humic acid-rectorite compound adsorbent 0.2g preparing under above-mentioned condition, and under room temperature, concussion absorption 20min, adopts the residual Pb of atomic absorption spectroscopy determination
2+concentration is 0.7mg/L, Pb
2+clearance reaches 98.6%.
Embodiment 2:
Take 8 parts of rectorites and add in 120 parts of water and be mixed with rectorite water slurry, then add 0.5 part of softex kw, regulate pH value to 6.5, stirring reaction 20h under 70 ℃ of water-baths, product washs by a large amount of deionized waters, until noresidue Br
-till, dry, be ground to 180 orders, obtain the rectorite that organises.Take 1.0 parts of acrylic acid, add in 20 parts of deionized waters, dissolve.Then under ice-water bath condition, add 0.3 part of NaOH, stirring reaction 15min.Aforesaid propylene aqueous acid is transferred in four-hole boiling flask, at N
2under protection, add 2 parts of organic rectorites and 0.1 part of humic acid, fully stir 10min; then slowly add 0.003 part of crosslinking agent N, N '-methylene-bisacrylamide and 0.01 part of initiator potassium persulfate, by warming-in-water to 40 ℃; prepolymerization 25min, is then warming up to 70 ℃ of reaction 2h.After reaction finishes, product is fully washed with ethanol, dry at 70 ℃, be ground to 200 orders, obtain polyacrylic acid-humic acid-rectorite compound adsorbent.
Configure respectively the Cd that 1.0L concentration is 50mg/L
2+, Cu
2+, Zn
2+solution, adds respectively the polyacrylic acid-humic acid-rectorite compound adsorbent 0.5g preparing under above-mentioned condition, and under room temperature, concussion absorption 30min, adopts the residual Cd of atomic absorption spectroscopy determination
2+, Cu
2+, Zn
2+concentration, calculates Cd
2+, Cu
2+, Zn
2+clearance be respectively 97.5%, 98.0% and 88.5%.
Embodiment 3:
Take 12 parts of rectorites and add in 120 parts of water and be mixed with rectorite water slurry, then add 1.5 parts of softex kws, regulate pH value to 6.0, stirring reaction 24h under 70 ℃ of water-baths, product washs by a large amount of deionized waters, until noresidue Br
-till, dry, be ground to 240 orders, obtain the rectorite that organises.Take 1.2 parts of acrylic acid, add in 24 parts of deionized waters, dissolve.Then under ice-water bath condition, add 0.6 part of NaOH, stirring reaction 20min.Aforesaid propylene aqueous acid is transferred in four-hole boiling flask, at N
2under protection; add 2.4 parts of organic rectorites and 0.3 part of humic acid; fully stir 10min; then slowly add 0.008 part of crosslinking agent N; N '-methylene-bisacrylamide and 0.04 part of initiator potassium persulfate; by warming-in-water to 40 ℃, prepolymerization 30min, is then warming up to 75 ℃ of reaction 2.5h.After reaction finishes, product is fully washed with ethanol, dry at 70 ℃, be ground to 200 orders, obtain polyacrylic acid-humic acid-rectorite compound adsorbent.
Configuration 1.0L concentration is respectively anthracene and the luxuriant and rich with fragrance solution of 1.0mg/L and 0.1mg/L, add respectively the polyacrylic acid-humic acid-rectorite compound adsorbent 2.0g preparing under above-mentioned condition, concussion absorption 180min under room temperature, employing gas chromatography determination anthracene and luxuriant and rich with fragrance residual concentration, calculate anthracene and luxuriant and rich with fragrance clearance is respectively 81.5% and 74.0%.
Embodiment 4:
Take 15 parts of rectorites and add in 150 parts of water and be mixed with rectorite water slurry, then add 1.8 parts of TTABs, regulate pH value to 6.5, stirring reaction 24h under 70 ℃ of water-baths, product washs by a large amount of deionized waters, until noresidue Br
-till, dry, be ground to 200 orders, obtain the rectorite that organises.Take 1.5 parts of acrylic acid, add in 30 parts of deionized waters, dissolve.Then under ice-water bath condition, add 0.8 part of NaOH, stirring reaction 20min.Aforesaid propylene aqueous acid is transferred in four-hole boiling flask, at N
2under protection; add 2.8 parts of organic rectorites and 0.5 part of humic acid; fully stir 10min; then slowly add 0.01 part of crosslinking agent N; N '-methylene-bisacrylamide and 0.05 part of initiator potassium persulfate; by warming-in-water to 40 ℃, prepolymerization 35min, is then warming up to 80 ℃ of reaction 3.0h.After reaction finishes, product is fully washed with ethanol, dry at 70 ℃, be ground to 200 orders, obtain polyacrylic acid-humic acid-rectorite compound adsorbent.
Configuration 1.0LPb
2+with luxuriant and rich with fragrance mixed solution, Pb in mixed solution
2+be respectively 50mg/L and 1.0mg/L with luxuriant and rich with fragrance concentration.In mixed solution, add the compound adsorbent of preparing under the above-mentioned condition of 2.0g, under room temperature, vibration absorption 120min, adopts respectively Pb in atomic absorption spectrophotometry and gas chromatography determination solution
2+residual concentration with luxuriant and rich with fragrance, calculates Pb
2+be respectively 98.2% and 80.9% with luxuriant and rich with fragrance clearance.
Thermogravimetric analysis shows, below 328.5 ℃, the adsorbent of preparation is obviously not weightless, good thermal stability; Use dilute acid soln and methanol aqueous solution can make respectively the desorb from adsorbent of heavy metal ion and polycyclic aromatic hydrocarbon, the adsorbent after regeneration is also reusable.
Claims (4)
1. a preparation method for polyacrylic acid-humic acid-rectorite compound adsorbent, is characterized in that comprising the following steps:
(1) preparation of organic rectorite: 5 ~ 15 parts of rectorites are added in 50 ~ 150 parts of water, stir, be mixed with rectorite water slurry, add 0.5 ~ 2 part of quaternary ammonium salt, regulate pH value to 5.5 ~ 6.5, and under 60 ~ 70 ℃ of water-baths stirring reaction 18 ~ 24h, then wash by deionized water, until the halide ion of noresidue, and through super-dry, be ground to 180 ~ 240 orders, obtain organic rectorite;
(2) preparation of acrylic acid aqueous solution and neutralization: take 1.0 ~ 1.5 parts of acrylic acid, add in 20 ~ 30 parts of deionized waters, dissolve; Then add 0.3 ~ 0.8 part of NaOH, stirring reaction 10 ~ 20min;
(3) polymerisation: the acrylic acid aqueous solution that step (2) is obtained is transferred in reaction vessel, and under the protection of inert gas, add 2 ~ 3 parts of organic rectorites and 0.1 ~ 0.5 part of humic acid, fully stir 10min, slowly add 0.002 ~ 0.01 part of crosslinking agent and 0.01 ~ 0.05 part of initator, temperature is risen to 40 ~ 50 ℃, and prepolymerization 25 ~ 40min, is then warming up to 60 ~ 80 ℃ of reaction 2 ~ 3h;
(4) product of (3) step is fully washed with ethanol, then dry at 70 ~ 85 ℃, be ground to 180 ~ 240 orders, obtain polyacrylic acid-humic acid-rectorite compound adsorbent;
In above-mentioned preparation process, the umber of each material is mass fraction.
2. the preparation method of polyacrylic acid-humic acid-rectorite compound adsorbent according to claim 1, is characterized in that: described quaternary ammonium salt is any one in softex kw, cetalkonium chloride, TTAB, myristyl dimethyl benzyl ammonium chloride or dodecyl benzyl dimethyl ammonium chloride.
3. the preparation method of polyacrylic acid-humic acid-rectorite compound adsorbent according to claim 1, is characterized in that: described crosslinking agent is N, N '-methylene-bisacrylamide.
4. the preparation method of polyacrylic acid-humic acid-rectorite compound adsorbent according to claim 1, is characterized in that: described initator is potassium peroxydisulfate.
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