CN102658100A - 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 the material for water treatment technical field, relate to a kind of preparation technology of organic/inorganic compound adsorbent specifically.
Background technology
Heavy metal and polycyclic aromatic hydrocarbon are the persistent pollutants of two quasi-representatives in the environment, are the research focuses of field of environment engineering to heavy metal and polycyclic aromatic hydrocarbons contaminated improvement therefore.Absorption method is adopted in heavy metal and polycyclic aromatic hydrocarbons contaminated improvement usually, and the adsorbent that uses in the industry mainly is active carbon and macromolecule polymeric adsorbent, but these two types of adsorbents cost an arm and a leg, and regeneration is difficult, has limited its application to a certain extent.In recent years; Exploitation to cheap and the adsorbent that adsorption efficiency is high is the research focus of field of waste water treatment always; Yet; Present research and development to sorbing material, only to single heavy metal or single polycyclic aromatic hydrocarbon, the someone develops the adsorbent that can efficiently adsorb heavy metal and polycyclic aromatic hydrocarbon simultaneously as yet.In fact, heavy metal and polycyclic aromatic hydrocarbon form heavy metal and polycyclic aromatic hydrocarbon combined pollution often simultaneously or successively get in the environment.Contain a large amount of heavy metals and polycyclic aromatic hydrocarbon in the creasote like the use of timber preservative factory, they can be detected in environment usually simultaneously.At present, China's surface water body generally receives the combined pollution of heavy metal and polycyclic aromatic hydrocarbon, like Taihu Lake basin, and South Lake, Changchun etc., wherein, heavy metal lead, cadmium, copper, zinc and polycyclic aromatic hydrocarbon fluorenes, phenanthrene, anthracene, pyrene all detect in the South Lake water body.Chemical interaction can take place in heavy metal in the environment and polycyclic aromatic hydrocarbon, and as forming heavy metal organic complex etc., these complex compounds will produce more complex environment effect with respect to single pollutant, causes more serious environmental pollution.Therefore; The improvement of heavy metal-polycyclic aromatic hydrocarbon combined pollution will more and more receive people's attention, and it is significant for the reparation of heavy metal and polycyclic aromatic hydrocarbon combined pollution water body to develop a kind of sorbing material that can remove heavy metal ion and multiring aromatic hydrocarbon substance simultaneously.
In recent years; Along with composite organic-inorganic material going deep in the application study in each field; It is feedstock production polyalcohol/clay soil composite adsorbing material that existing researcher adopts organic matter and inorganic clay, because the introducing of inorganic component has reduced the preparation of adsorbent cost.Yet the polyalcohol/clay soil composite adsorbing material of having developed is mainly used in the strong heavy metal ion of absorption hydrophily and the dye of positive ion etc., can not adsorb hydrophobic organic pollutant, like polycyclic aromatic hydrocarbon etc.
Summary of the invention
Goal of the invention: to the problem and shortage of above-mentioned existing existence; The preparation method who the purpose of this invention is to provide a kind of polyacrylic acid-humic acid-rectorite compound adsorbent; This adsorbent has excellent absorption property simultaneously to heavy metal in the water and polyaromatic hydrocarbon pollutant; Overcome existing polyalcohol/clay soil composite adsorbing material and only be used to adsorb the strong heavy metal ion of hydrophily and the dye of positive ion etc.; The drawback that can not adsorb hydrophobic organic pollutant is for the improvement of heavy metal and polycyclic aromatic hydrocarbon combined pollution provides new material.
Technical scheme: for realizing the foregoing invention purpose, the present invention adopts following technical scheme: the preparation method of a kind of polyacrylic acid-humic acid-rectorite compound adsorbent is characterized in that may further comprise the steps:
(1) preparation of organic rectorite: 5 ~ 15 parts of rectorites are added in 50 ~ 150 parts of water, stir, be mixed with the 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; Spend deionised water then; Till 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 by weighing 1.0 ~ 1.5 parts of acrylic acid, add in 20 ~ 30 parts of deionized waters, dissolving; Add 0.3 ~ 0.8 part of NaOH then, stirring reaction 10 ~ 20min;
(3) polymerisation: the acrylic acid aqueous solution that step (2) is obtained is transferred in the 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 reaction 25 ~ 40min is warming up to 60 ~ 80 ℃ of reaction 2 ~ 3h then;
(4) product with (3) step fully washs with ethanol, and is dry under 70 ~ 85 ℃ then, is ground to 180 ~ 240 orders, obtains polyacrylic acid-humic acid-rectorite compound adsorbent;
In the above-mentioned preparation process, the umber of each material is mass fraction.
As preferably, said quaternary ammonium salt is any one in softex kw, cetalkonium chloride, TTAB, myristyl dimethyl benzyl ammonium chloride or the dodecyl benzyl dimethyl ammonium chloride.
As preferably, said crosslinking agent is N, N '-methylene-bisacrylamide; Said initator is a 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 humic acid to the good adsorption capacity of polycyclic aromatic hydrocarbon and the polyacrylic acid efficient adsorption capacity to heavy metal; Make the adsorbent of invention can adsorb heavy metal and polycyclic aromatic hydrocarbon simultaneously; 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 adsorption site that the rectorite interlamellar spacing increases, hydrophobicity strengthens, increase is new, the adsorbent of feasible preparation improves the adsorption capacity of hydrophobic organic compound, adds the absorption of humic acid to polycyclic aromatic hydrocarbon; Make this adsorbent in the efficient absorption that guarantees heavy metal; Polycyclic aromatic hydrocarbon also there is the good adsorption effect, has overcome similar adsorbent and can only adsorb heavy metal, can not adsorb the drawback of hydrophobic contaminant; (3) heavy metal class and polyaromatic hydrocarbon pollutant on this adsorbent adsorption mechanism different with the adsorption site position; There is not competitive Adsorption; Can use this adsorbent efficient heavy metal and polycyclic aromatic hydrocarbon removed from water simultaneously, be used for containing simultaneously the wastewater treatment of heavy metal and polycyclic aromatic hydrocarbon and receive polycyclic aromatic hydrocarbon and the reparation of heavy-metal composite pollution water body; (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 only be used to the present invention is described and be not used in the restriction scope of the present invention; After having read the present invention, those skilled in the art all fall within the application's accompanying claims institute restricted portion to the modification of the various equivalent form of values of the present invention.
Because the polyacrylic acid resinoid has higher adsorption capacity to the heavy metal in the water; And adsorption rate is fast; Rectorite mineral and humic acid all have the good adsorption ability to heavy metal and polycyclic aromatic hydrocarbon; With the composite synthetic compound adsorbent of acrylic acid, humic acid and rectorite; Can make full use of rectorite and humic acid to the good adsorption capacity of polycyclic aromatic hydrocarbon and polyacrylic acid efficient adsorption capacity to heavy metal, the fast advantage of performance polyacrylic resin adsorption rate, heavy metal and polycyclic aromatic hydrocarbon in the water are removed in absorption fast simultaneously.Adopt organic quaternary ammonium salt and rectorite generation cation exchange reaction to form organic rectorite; Make the acrylic acid in-situ polymerization then between the nanometer layer of organic rectorite; Form intercal type polyalcohol/clay soil composite; Humic acid in the load simultaneously makes polyacrylic acid-humic acid-rectorite compound adsorbent.
Embodiment 1:
Take by weighing in 100 parts of water of 10 parts of rectorites addings and be mixed with the rectorite water slurry, add 1.0 parts of softex kws again, regulate pH value to 6.5, stirring reaction 24h under 70 ℃ of water-baths, product washs with a large amount of deionized waters, up to noresidue Br
-Till, drying is ground to 200 orders, obtains organic rectorite.Take by weighing 1.2 parts of acrylic acid, add in 25 parts of deionized waters, dissolving.Under the ice-water bath condition, add 0.5 part of NaOH, stirring reaction 10min then.The aforesaid propylene aqueous acid is transferred in the four-hole boiling flask, at N
2Protection adds 2.6 parts of organic rectorites and 0.2 part of humic acid down, fully stirs 10min; Slowly add 0.005 part of crosslinking agent N then, N '-methylene-bisacrylamide and 0.03 part of initiator potassium persulfate are with warming-in-water to 40 ℃; Prepolymerization reaction 30min is warming up to 70 ℃ of reaction 3h then.Reaction is fully washed product with ethanol after finishing, and is dry under 70 ℃, is ground to 200 orders, obtains polyacrylic acid-humic acid-rectorite compound adsorbent.
Configuration 1.0L concentration is the Pb of 50mg/L
2+Solution adds the polyacrylic acid-humic acid-rectorite compound adsorbent 0.2g for preparing under the above-mentioned condition, and concussion absorption 20min adopts the residual Pb of atomic absorption spectroscopy determination under the room temperature
2+Concentration is 0.7mg/L, Pb
2+Clearance reaches 98.6%.
Embodiment 2:
Take by weighing in 120 parts of water of 8 parts of rectorites addings and be mixed with the rectorite water slurry, add 0.5 part of softex kw again, regulate pH value to 6.5, stirring reaction 20h under 70 ℃ of water-baths, product washs with a large amount of deionized waters, up to noresidue Br
-Till, drying is ground to 180 orders, obtains the rectorite that organises.Take by weighing 1.0 parts of acrylic acid, add in 20 parts of deionized waters, dissolving.Under the ice-water bath condition, add 0.3 part of NaOH, stirring reaction 15min then.The aforesaid propylene aqueous acid is transferred in the four-hole boiling flask, at N
2Protection adds 2 parts of organic rectorites and 0.1 part of humic acid down, fully stirs 10min; Slowly add 0.003 part of crosslinking agent N then, N '-methylene-bisacrylamide and 0.01 part of initiator potassium persulfate are with warming-in-water to 40 ℃; Prepolymerization reaction 25min is warming up to 70 ℃ of reaction 2h then.Reaction is fully washed product with ethanol after finishing, and is dry under 70 ℃, is ground to 200 orders, obtains polyacrylic acid-humic acid-rectorite compound adsorbent.
Dispose the Cd that 1.0L concentration is 50mg/L respectively
2+, Cu
2+, Zn
2+Solution adds the polyacrylic acid-humic acid-rectorite compound adsorbent 0.5g for preparing under the above-mentioned condition respectively, and concussion absorption 30min adopts the residual Cd of atomic absorption spectroscopy determination under the room temperature
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 by weighing in 120 parts of water of 12 parts of rectorites addings and be mixed with the rectorite water slurry, add 1.5 parts of softex kws again, regulate pH value to 6.0, stirring reaction 24h under 70 ℃ of water-baths, product washs with a large amount of deionized waters, up to noresidue Br
-Till, drying is ground to 240 orders, obtains the rectorite that organises.Take by weighing 1.2 parts of acrylic acid, add in 24 parts of deionized waters, dissolving.Under the ice-water bath condition, add 0.6 part of NaOH, stirring reaction 20min then.The aforesaid propylene aqueous acid is transferred in the four-hole boiling flask, at N
2Protection down; Add 2.4 parts of organic rectorites and 0.3 part of humic acid, fully stir 10min, slowly add 0.008 part of crosslinking agent N then; N '-methylene-bisacrylamide and 0.04 part of initiator potassium persulfate; With warming-in-water to 40 ℃, prepolymerization reaction 30min is warming up to 75 ℃ of reaction 2.5h then.Reaction is fully washed product with ethanol after finishing, and is dry under 70 ℃, is ground to 200 orders, obtains 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 the polyacrylic acid-humic acid-rectorite compound adsorbent 2.0g for preparing under the above-mentioned condition respectively; Concussion absorption 180min under the room temperature; Adopt gas chromatography determination anthracene and luxuriant and rich with fragrance residual concentration, calculate anthracene and be respectively 81.5% and 74.0% with luxuriant and rich with fragrance clearance.
Embodiment 4:
Take by weighing in 150 parts of water of 15 parts of rectorites addings and be mixed with the rectorite water slurry, add 1.8 parts of TTABs again, regulate pH value to 6.5, stirring reaction 24h under 70 ℃ of water-baths, product washs with a large amount of deionized waters, up to noresidue Br
-Till, drying is ground to 200 orders, obtains the rectorite that organises.Take by weighing 1.5 parts of acrylic acid, add in 30 parts of deionized waters, dissolving.Under the ice-water bath condition, add 0.8 part of NaOH, stirring reaction 20min then.The aforesaid propylene aqueous acid is transferred in the four-hole boiling flask, at N
2Protection down; Add 2.8 parts of organic rectorites and 0.5 part of humic acid, fully stir 10min, slowly add 0.01 part of crosslinking agent N then; N '-methylene-bisacrylamide and 0.05 part of initiator potassium persulfate; With warming-in-water to 40 ℃, prepolymerization reaction 35min is warming up to 80 ℃ of reaction 3.0h then.Reaction is fully washed product with ethanol after finishing, and is dry under 70 ℃, is ground to 200 orders, obtains polyacrylic acid-humic acid-rectorite compound adsorbent.
Configuration 1.0LPb
2+With the mixed solution of phenanthrene, Pb in the 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 for preparing under the above-mentioned condition of 2.0g, vibration absorption 120min adopts Pb in atomic absorption spectrophotometry and the gas chromatography determination solution respectively under the room temperature
2+Residual concentration with phenanthrene calculates Pb
2+Be respectively 98.2% and 80.9% with the clearance of phenanthrene.
Thermogravimetric analysis shows that below 328.5 ℃, the adsorbent of preparation is obviously not weightless, good thermal stability; Use dilute acid soln and methanol aqueous solution can make the desorb from the adsorbent of heavy metal ion and polycyclic aromatic hydrocarbon respectively, the adsorbent after the regeneration is also reusable.
Claims (4)
1. the preparation method of polyacrylic acid-humic acid-rectorite compound adsorbent is characterized in that may further comprise the steps:
(1) preparation of organic rectorite: 5 ~ 15 parts of rectorites are added in 50 ~ 150 parts of water, stir, be mixed with the 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; Spend deionised water then; Till 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 by weighing 1.0 ~ 1.5 parts of acrylic acid, add in 20 ~ 30 parts of deionized waters, dissolving; Add 0.3 ~ 0.8 part of NaOH then, stirring reaction 10 ~ 20min;
(3) polymerisation: the acrylic acid aqueous solution that step (2) is obtained is transferred in the 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 reaction 25 ~ 40min is warming up to 60 ~ 80 ℃ of reaction 2 ~ 3h then;
(4) product with (3) step fully washs with ethanol, and is dry under 70 ~ 85 ℃ then, is ground to 180 ~ 240 orders, obtains polyacrylic acid-humic acid-rectorite compound adsorbent;
In the above-mentioned preparation process, the umber of each material is mass fraction.
2. according to the preparation method of the said polyacrylic acid-humic acid of claim 1-rectorite compound adsorbent, it is characterized in that: said quaternary ammonium salt is any one in softex kw, cetalkonium chloride, TTAB, myristyl dimethyl benzyl ammonium chloride or the dodecyl benzyl dimethyl ammonium chloride.
3. according to the preparation method of the said polyacrylic acid-humic acid of claim 1-rectorite compound adsorbent, it is characterized in that: said crosslinking agent is N, N '-methylene-bisacrylamide.
4. according to the preparation method of the said polyacrylic acid-humic acid of claim 1-rectorite compound adsorbent, it is characterized in that: said initator is a potassium peroxydisulfate.
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