CN109772274A - Mercury-containing waste water treatment method - Google Patents
Mercury-containing waste water treatment method Download PDFInfo
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- CN109772274A CN109772274A CN201910077668.9A CN201910077668A CN109772274A CN 109772274 A CN109772274 A CN 109772274A CN 201910077668 A CN201910077668 A CN 201910077668A CN 109772274 A CN109772274 A CN 109772274A
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Abstract
The invention discloses a kind of mercury-containing waste water treatment methods.Adsorbent material is placed in mercury-containing waste water by this method, and stirring 6 hours or more to realize the processing to mercury-containing waste water;The adsorbent material is prepared by the following method: by ZIF-67 and polyacrylic acid in N, ultrasound to scattering completely in dinethylformamide, molysite, manganese salt, sodium selenate and urea are dissolved in above-mentioned solution under ultrasound condition again, ultrasound is until system is evenly dispersed, the dispersion liquid is subjected to hydro-thermal reaction, it is filtered, washed, dries, obtain product A, product A is dispersed in DMF, by N, N- Dicyclohexylcarbodiimide, polyacrylamide solution are added thereto, after ultrasonic disperse, it is stirred to react at room temperature, obtains the adsorbent material.The present invention, which uses, uses selectivity high, and adsorption capacity is big, environmentally friendly magnetic adsorptive material, can handle the low concentration mercury-containing waste water of 50 ~ 100mg/L, adsorption efficiency can reach 98%, and can be recycled.
Description
Technical field
The present invention relates to a kind of mercury-containing waste water treatment method, especially a kind of low concentration mercury-containing waste water treatment method belongs to
Technical field of waste water processing.
Background technique
China's water body mercury pollution faces various problems, the mercury concentration over-standard in many basins.Harmful mercury metallic pollution waste water is
One of the important environmental problem that current China is faced.The processing method of mercury metallic wastewater mainly has chemical precipitation, novel suction
Attached dose of absorption, UF membrane, electrochemical process, photocatalysis, bio-flocculation process etc..Wherein, absorption method is because of easy to operate, treatment effeciency
Height becomes the most-often used method that mercury metal ion removes in actual waste water.
Absorption method is mild with operating condition, has wide range of applications, does not introduce new impurity, can carry out depth to waste water
The advantages that processing and widely studied.Currently, the adsorbent research based on active carbon is more, it may have preferable absorption
Effect, but due in practical water body pollutant kind it is more, and mercury concentration is not high, and active carbon is in adsorptive selectivity and absorption
It is still had several drawbacks in depth.
Summary of the invention
The object of the present invention is to provide a kind of mercury-containing waste water treatment methods.
Realizing the technical solution of the object of the invention is: a kind of mercury absorbent by metal-organic framework materials ZIF-67 and gathers
Ultrasound to scattering completely in n,N-Dimethylformamide for acrylic acid, then by molysite, manganese salt, sodium selenate and urea in ultrasound condition
Under be successively dissolved in above-mentioned solution, ultrasound until system it is evenly dispersed, it is anti-that which is carried out to hydro-thermal at 120~200 DEG C
It answers, is filtered, washed, dries, obtain product A, product A is dispersed in DMF, by N, N- Dicyclohexylcarbodiimide, polypropylene
Amide solution is added thereto, and after ultrasonic disperse, is stirred to react at room temperature, and the adsorbent material is obtained.
Further, concentration of the ZIF-67 in n,N-Dimethylformamide is 2~5g/L, ZIF-67 and polyacrylic acid with
The mass ratio of molysite is 1:4~6:5~6.
Further, the molar ratio of molysite, manganese salt, sodium selenate and urea is 2:1:0.5~2:8~12.
Further, the time of hydro-thermal reaction is 10~15h.
Further, the mass ratio of N, N- Dicyclohexylcarbodiimide and polyacrylamide is 5~20:1.
Further, the mass ratio of polyacrylamide and ZIF-67 are 0.5~1:1.
By the application of above-mentioned mercury absorbent mercury metal in absorption waste water.
Further, the mass concentration of waste water metal mercury is not less than 50mg/L.
Further, the mass concentration of mercury metal is not less than 100mg/L in waste water.
Further, the pH value of waste water is between 5~10.
Further, the mass ratio of mercury absorbent and waste water is 0.05~0.5g/100ml.
Further, the time of mercury absorbent absorption waste water is 6 hours or more, preferably 10 hours or more.
Compared with prior art, the invention has the advantages that
(1) present invention is using the metal-organic framework materials ZIF-67 of large specific surface area as carrier, using precipitating-hydro-thermal reaction
In conjunction with method, using on the Manganese Ferrite for the being doped with selenium carrier evenly dispersed as active component, while using polyacrylic acid pair
Active component is modified, then polyacrylamide is grafted, and obtains a kind of selectivity height, adsorption capacity is big, environmentally friendly magnetic
Property adsorbent material, have very well dispersibility, have preferable adsorption effect to mercury, can be recycled.
(2) present invention solves the problem that adsorbent material is easy to reunite in waste water, is not easily recycled, and the adsorbent material energy
It is recycled.
(3) adsorbent material of the present invention has preferable stability, can stablize under the higher state of temperature
In the presence of.
(4) adsorbent material of the present invention can handle low concentration wastewater (50~100mg/L), and adsorption efficiency can reach
98%.
Detailed description of the invention
Fig. 1 is the circulation absorption experimental result picture of adsorbent material of the present invention.
Specific embodiment
The preparation of embodiment 1:ZIF-67
Co(NO3)2·6H2O 291mg and 2-methylimidazole 328mg, which is dissolved separately in 25ml methanol solution, to be mixed, room temperature
Lower stirring for 24 hours, to be centrifuged 5min in 6000rpm after reaction, with ethanol washing 4 times, obtains the drying at 60 DEG C after solid phase
6h forms ZIF-67.
Embodiment 2:MnFe2O4The preparation of/ZIF-67 adsorbent material
It weighs 100mg ZIF-67 and is added to 50mlN, in dinethylformamide, ultrasonic 30min keeps system dispersion equal
It is even；Again by 2mmol FeCl3.6H2O、1mmol MnCl2, 0.48g urea above-mentioned solution is successively dissolved under ultrasound condition, ultrasound
30min is sufficiently mixed system, evenly dispersed；It is high-pressure sealed anti-that this solution is then transferred to 150ml stainless steel polytetrafluoroethylene (PTFE)
It answers in kettle, 200 DEG C of constant temperature 12h in constant temperature oven；Repeatedly washed with deionized water and ethyl alcohol, with vacuum drying oven 323K item
Dry 12h, obtains product 1 under part.
The MnFe of embodiment 3:Se doping2O4The preparation of/ZIF-67 adsorbent material
It weighs 100mg ZIF-67 and is added to 50mlN, in dinethylformamide, ultrasonic 30min keeps system dispersion equal
It is even；Again by 2mmol FeCl3.6H2O、1mmol MnCl2、0.5mmol Na2SeO4, 0.5g urea it is successively molten under ultrasound condition
In above-mentioned solution, ultrasonic 30min is sufficiently mixed system, evenly dispersed；This solution is then transferred to 150ml stainless steel poly- four
In the high-pressure sealed reaction kettle of vinyl fluoride, 200 DEG C of constant temperature 12h in constant temperature oven；It is repeatedly washed with deionized water and ethyl alcohol, with true
Empty baking oven dry 12h under conditions of 323K, obtains product 2.
The MnFe of embodiment 4:Se doping2O4The preparation of/ZIF-67- polyacrylic acid adsorbent material
It weighs 100mg ZIF-67 and 400mg polyacrylic acid and is added to 50mlN, in dinethylformamide, ultrasound
30min makes system be uniformly dispersed；Again by 2mmol FeCl3.6H2O、1mmol MnCl2、0.5mmol Na2SeO4, 0.5g urea
Above-mentioned solution is successively dissolved under ultrasound condition, ultrasonic 30min is sufficiently mixed system, evenly dispersed；Then this solution is turned
Enter in the high-pressure sealed reaction kettle of 150ml stainless steel polytetrafluoroethylene (PTFE), 200 DEG C of constant temperature 12h in constant temperature oven；With deionized water and
Ethyl alcohol repeatedly washs, and dries 12h under conditions of 323K with vacuum drying oven, obtains product 3.
The MnFe of embodiment 5:Se doping2O4The preparation of/ZIF-67- poly acrylic acid-poly acrylamide adsorbent material
It weighs 100mg ZIF-67 and 400mg polyacrylic acid and is added to 50mlN, in dinethylformamide, ultrasound
30min makes system be uniformly dispersed；Again by 2mmol FeCl3.6H2O、1mmol MnCl2、0.5mmol Na2SeO4, 0.5g urea
Above-mentioned solution is successively dissolved under ultrasound condition, ultrasonic 30min is sufficiently mixed system, evenly dispersed；Then this solution is turned
Enter in the high-pressure sealed reaction kettle of 150ml stainless steel polytetrafluoroethylene (PTFE), 200 DEG C of constant temperature 12h in constant temperature oven；With deionized water and
Ethyl alcohol repeatedly washs, and dries 12h under conditions of 323K with vacuum drying oven, dried product exhibited is dispersed in DMF；Then will
(dried product exhibited in above-mentioned mixed solution is added in 500mg N, N- Dicyclohexylcarbodiimide, 30ml 2.5g/L polyacrylamide
The mixed solution of+DMF), after ultrasonic 15min, 12h is stirred at room temperature；After reaction magnet separate, and with ethyl alcohol and go from
The mixed liquor of sub- water repeatedly washs (V:V=1:1)；12h is dried under conditions of 323K with vacuum drying oven, obtains product 4.
The MnFe of embodiment 6:Se doping2O4The preparation of/ZIF-67- poly acrylic acid-poly acrylamide adsorbent material
It weighs 100mg ZIF-67 and 500mg polyacrylic acid to be added in 50ml n,N-Dimethylformamide, ultrasound
30min makes system be uniformly dispersed；Again by 2mmol FeCl3.6H2O、1mmol MnCl2、0.5mmol Na2SeO4, 0.5g urea
Above-mentioned solution is successively dissolved under ultrasound condition, ultrasonic 30min is sufficiently mixed system, evenly dispersed；Then this solution is turned
Enter in the high-pressure sealed reaction kettle of 150ml stainless steel polytetrafluoroethylene (PTFE), 200 DEG C of constant temperature 12h in constant temperature oven；With deionized water and
Ethyl alcohol repeatedly washs, and dries 12h under conditions of 323K with vacuum drying oven, dried product exhibited is dispersed in DMF；Then will
500mg N, N- Dicyclohexylcarbodiimide, 30ml 2.5g/L polyacrylamide are added in above-mentioned mixed solution, ultrasonic 15min
Afterwards, 12h is stirred at room temperature；Magnet separates after reaction, and repeatedly washs (V:V with ethyl alcohol and the mixed liquor of deionized water
=1:1)；12h is dried under conditions of 323K with vacuum drying oven, obtains product 5.
The MnFe of embodiment 7:Se doping2O4The preparation of/ZIF-67- poly acrylic acid-poly acrylamide adsorbent material
It weighs 100mg ZIF-67 and 600mg polyacrylic acid to be added in 50m n,N-Dimethylformamide, ultrasound
30min makes system be uniformly dispersed；Again by 2mmol FeCl3.6H2O、1mmol MnCl2、0.5mmol Na2SeO4, 0.5g urea
Above-mentioned solution is successively dissolved under ultrasound condition, ultrasonic 30min is sufficiently mixed system, evenly dispersed；Then this solution is turned
Enter in the high-pressure sealed reaction kettle of 150ml stainless steel polytetrafluoroethylene (PTFE), 200 DEG C of constant temperature 12h in constant temperature oven；With deionized water and
Ethyl alcohol repeatedly washs, and dries 12h under conditions of 323K with vacuum drying oven, dried product exhibited is dispersed in DMF；Then will
500mg N, N- Dicyclohexylcarbodiimide, 30ml 2.5g/L polyacrylamide are added in above-mentioned mixed solution, ultrasonic 15min
Afterwards, 12h is stirred at room temperature；Magnet separates after reaction, and repeatedly washs (V:V with ethyl alcohol and the mixed liquor of deionized water
=1:1)；12h is dried under conditions of 323K with vacuum drying oven, obtains product 6.
The MnFe of embodiment 8:Se doping2O4The preparation of/ZIF-67- poly acrylic acid-poly acrylamide adsorbent material
It weighs 100mg ZIF-67 and 500mg polyacrylic acid to be added in 50m n,N-Dimethylformamide, ultrasound
30min makes system be uniformly dispersed；Again by 2mmol FeCl3.6H2O、1mmol MnCl2、1mmol Na2SeO4, 0.5g urea exists
Above-mentioned solution is successively dissolved under ultrasound condition, ultrasonic 30min is sufficiently mixed system, evenly dispersed；Then this solution is transferred to
In the high-pressure sealed reaction kettle of 150ml stainless steel polytetrafluoroethylene (PTFE), 200 DEG C of constant temperature 12h in constant temperature oven；With deionized water and second
Alcohol repeatedly washs, and dries 12h under conditions of 323K with vacuum drying oven, dried product exhibited is dispersed in DMF；Then will
500mg N, N- Dicyclohexylcarbodiimide, 30ml 2.5g/L polyacrylamide are added in above-mentioned mixed solution, ultrasonic 15min
Afterwards, 12h is stirred at room temperature；Magnet separates after reaction, and repeatedly washs (V:V with ethyl alcohol and the mixed liquor of deionized water
=1:1)；12h is dried under conditions of 323K with vacuum drying oven, obtains product 7.
The MnFe of embodiment 9:Se doping2O4The preparation of/ZIF-67- poly acrylic acid-poly acrylamide adsorbent material
It weighs 100mg ZIF-67 and 500mg polyacrylic acid to be added in 50m n,N-Dimethylformamide, ultrasound
30min makes system be uniformly dispersed；Again by 2mmol FeCl3.6H2O、1mmol MnCl2、2mmol Na2SeO4, 0.5g urea exists
Above-mentioned solution is successively dissolved under ultrasound condition, ultrasonic 30min is sufficiently mixed system, evenly dispersed；Then this solution is transferred to
In the high-pressure sealed reaction kettle of 150ml stainless steel polytetrafluoroethylene (PTFE), 200 DEG C of constant temperature 12h in constant temperature oven；With deionized water and second
Alcohol repeatedly washs, and dries 12h under conditions of 323K with vacuum drying oven, dried product exhibited is dispersed in DMF；Then will
500mg N, N- Dicyclohexylcarbodiimide, 30ml 2.5g/L polyacrylamide are added in above-mentioned mixed solution, ultrasonic 15min
Afterwards, 12h is stirred at room temperature；Magnet separates after reaction, and repeatedly washs (V:V with ethyl alcohol and the mixed liquor of deionized water
=1:1)；12h is dried under conditions of 323K with vacuum drying oven, obtains product 8.
The MnFe of embodiment 10:Se doping2O4The preparation of/ZIF-67- poly acrylic acid-poly acrylamide adsorbent material
It weighs 100mg ZIF-67 and 500mg polyacrylic acid to be added in 50m n,N-Dimethylformamide, ultrasound
30min makes system be uniformly dispersed；Again by 2mmol FeCl3.6H2O、1mmol MnCl2、1mmol Na2SeO4, 0.5g urea exists
Above-mentioned solution is successively dissolved under ultrasound condition, ultrasonic 30min is sufficiently mixed system, evenly dispersed；Then this solution is transferred to
In the high-pressure sealed reaction kettle of 150ml stainless steel polytetrafluoroethylene (PTFE), 200 DEG C of constant temperature 12h in constant temperature oven；With deionized water and second
Alcohol repeatedly washs, and dries 12h under conditions of 323K with vacuum drying oven, dried product exhibited is dispersed in DMF；Then will
500mg N, N- Dicyclohexylcarbodiimide, 40ml 2.5g/L polyacrylamide are added in above-mentioned mixed solution, ultrasonic 15min
Afterwards, 12h is stirred at room temperature；Magnet separates after reaction, and repeatedly washs (V:V with ethyl alcohol and the mixed liquor of deionized water
=1:1)；12h is dried under conditions of 323K with vacuum drying oven, obtains product 9.
The MnFe of embodiment 11:Se doping2O4The preparation of/ZIF-67- poly acrylic acid-poly acrylamide adsorbent material
It weighs 100mg ZIF-67 and 500mg polyacrylic acid to be added in 50m n,N-Dimethylformamide, ultrasound
30min makes system be uniformly dispersed；Again by 2mmol FeCl3.6H2O、1mmol MnCl2、1mmol Na2SeO4, 0.5g urea exists
Above-mentioned solution is successively dissolved under ultrasound condition, ultrasonic 30min is sufficiently mixed system, evenly dispersed；Then this solution is transferred to
In the high-pressure sealed reaction kettle of 150ml stainless steel polytetrafluoroethylene (PTFE), 200 DEG C of constant temperature 12h in constant temperature oven；With deionized water and second
Alcohol repeatedly washs, and dries 12h under conditions of 323K with vacuum drying oven, dried product exhibited is dispersed in DMF；Then will
500mg N, N- Dicyclohexylcarbodiimide, 20ml 2.5g/L polyacrylamide are added in above-mentioned mixed solution, ultrasonic 15min
Afterwards, 12h is stirred at room temperature；Magnet separates after reaction, and repeatedly washs (V:V with ethyl alcohol and the mixed liquor of deionized water
=1:1)；12h is dried under conditions of 323K with vacuum drying oven, obtains product 10.
The test of Hg absorption property has been carried out to the adsorption production 1-10 prepared in above-described embodiment 2-11.Specific test side
Method is: preparing the Hg solution of 100mg/L, measures the conical flask that 50ml is respectively placed in 100ml with pipette, adjusting pH value is 5 left
The right side is separately added into above-mentioned adsorbent material 0.05g into 10 conical flasks, and 10h, magnet point are stirred at 30 DEG C with constant temperature oscillator
From a small amount of supernatant is taken, unadsorbed Hg concentration is detected with Atomic absorption.Experimental data is as shown in table 1.Adsorption efficiency=(Hg
Residual concentration after initial concentration-absorption)/Hg initial concentration.
Table 1
Hg absorption property in waste water is carried out to the adsorption production 8 prepared in above-described embodiment 8 to test.Specific test side
Method is: take 100ml waste water (mercury content 100mg/L) to be placed in 200ml conical flask respectively, adjust pH value be respectively 5,6,7,8,
9,10,11, it is separately added into above-mentioned adsorbent material 0.1g into 7 conical flasks, stirs 10h, magnetic at 30 DEG C with constant temperature oscillator
Iron separation takes a small amount of supernatant, and unadsorbed Hg concentration is detected with Atomic absorption.Experimental data is as shown in table 2.
Table 2
Hg absorption property in waste water is carried out to the adsorption production 8 prepared in above-described embodiment 8 to test.Specific test side
Method is: taking 100ml waste water (mercury content 100mg/L) to be placed in 6 200ml conical flasks respectively, adjusting pH value is 7 or so, to 6
It is separately added into above-mentioned adsorbent material 0.01g, 0.05g, 0.1g, 0.3g, 0.5g, 1.0g in a conical flask, is existed with constant temperature oscillator
10h is stirred at 30 DEG C, magnet separation takes a small amount of supernatant, unadsorbed Hg concentration is detected with Atomic absorption.Experimental data is such as
Shown in table 3.
Table 3
Hg absorption property in waste water is carried out to the adsorption production 8 prepared in above-described embodiment 8 to test.Specific test side
Method is: take 100ml waste water respectively, wherein mercury content be respectively 20mg/L, 40mg/L, 50mg/L, 100mg/L, 200mg/L,
1000mg/L is placed in 6 200ml conical flasks, and adjusting pH value is 7 or so, is separately added into above-mentioned adsorption material into 6 conical flasks
Expect 0.5g, stir 10h at 30 DEG C with constant temperature oscillator, magnet separation takes a small amount of supernatant, is not inhaled with Atomic absorption detection
Attached Hg concentration.Experimental data is as shown in table 4.
Table 4
Hg absorption property in waste water is carried out to the adsorption production 8 prepared in above-described embodiment 8 to test.Specific test side
Method is: taking 100ml waste water (mercury content 100mg/L) to be placed in 5 200ml conical flasks respectively, adjusting pH value is 7 or so, to 5
Above-mentioned adsorbent material 0.1g is separately added into a conical flask, stirred respectively at 30 DEG C with constant temperature oscillator 4h, 6h, 8h, 10h,
12h, magnet separation take a small amount of supernatant, unadsorbed Hg concentration are detected with Atomic absorption.Experimental data is as shown in table 5.
Table 5
Fig. 1 is to be tested using the embodiment of the present invention 8 i.e. circulation absorption of product 7, there it can be seen that being repeated 5 times absorption
After Hg solution, its adsorption efficiency can still keep 96% or more after sorption cycle, illustrate that adsorbent material prepared by the present invention can
To reuse well.
Claims (10)
1. a kind of mercury-containing waste water treatment method, which is characterized in that adsorbent material is placed in mercury-containing waste water, stirring 6 hours or more;
The adsorbent material is prepared by the following method: metal-organic framework materials ZIF-67 and polyacrylic acid are in N, N- dimethyl
Ultrasound is successively dissolved in above-mentioned solution to scattering completely, then by molysite, manganese salt, sodium selenate and urea under ultrasound condition in formamide
In, ultrasound is evenly dispersed up to system, which is carried out hydro-thermal reaction at 120 ~ 200 DEG C, is filtered, washed, dries, obtain
To product A, product A is dispersed in DMF, by N, N- Dicyclohexylcarbodiimide, polyacrylamide solution are added thereto, ultrasound
It after dispersion, is stirred to react at room temperature, obtains the adsorbent material.
2. the method as described in claim 1, which is characterized in that concentration of the ZIF-67 in n,N-Dimethylformamide is 2 ~ 5
g/L。
3. the method as described in claim 1, which is characterized in that the mass ratio of ZIF-67 and polyacrylic acid and molysite is 1:4 ~ 6:
5~6。
4. the method as described in claim 1, which is characterized in that molysite, manganese salt, the molar ratio of sodium selenate and urea are 2:1:
0.5~2:8~12。
5. the method as described in claim 1, which is characterized in that the time of hydro-thermal reaction is 10 ~ 15 h.
6. the method as described in claim 1, which is characterized in that the quality of N, N- Dicyclohexylcarbodiimide and polyacrylamide
Than for 5 ~ 20:1.
7. the method as described in claim 1, which is characterized in that the mass ratio of polyacrylamide and ZIF-67 are 0.5 ~ 1:1.
8. the method as described in claim 1, which is characterized in that the mass concentration of waste water metal mercury is not less than 50 mg/L, most
It is not less than 100 mg/L well.
9. the method as described in claim 1, which is characterized in that the pH value of waste water is between 5 ~ 10, preferably between 7 ~ 9.
10. the method as described in claim 1, which is characterized in that the mass ratio of mercury absorbent and waste water is 0. 05 ~ 0.5g/
100ml。
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