CN111453875A - Water treatment method for N-nitrosodimethylamine in ferroferric oxide reinforced zero-valent iron reduction water - Google Patents

Water treatment method for N-nitrosodimethylamine in ferroferric oxide reinforced zero-valent iron reduction water Download PDF

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Publication number
CN111453875A
CN111453875A CN202010131012.3A CN202010131012A CN111453875A CN 111453875 A CN111453875 A CN 111453875A CN 202010131012 A CN202010131012 A CN 202010131012A CN 111453875 A CN111453875 A CN 111453875A
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ferroferric oxide
nitrosodimethylamine
zero
valent iron
ndma
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韩莹
吴越
黄俊恺
刘宏远
张克敏
吴召
陆青杰
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Zhejiang University of Technology ZJUT
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Zhejiang University of Technology ZJUT
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00—Multistage treatment of water, waste water or sewage
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/70—Treatment of water, waste water, or sewage by reduction
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/70—Treatment of water, waste water, or sewage by reduction
    • C02F1/705—Reduction by metals
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/26—Treatment of water, waste water, or sewage by extraction
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/38—Organic compounds containing nitrogen

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  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Compounds Of Iron (AREA)

Abstract

The invention discloses a water treatment method of N-nitrosodimethylamine in ferroferric oxide reinforced zero-valent iron reduction water, which comprises the steps of adjusting the pH value of a buffer solution, adding the buffer solution into an extraction device, adding iron powder, ferroferric oxide and NDMA mother solution into the extraction device, preparing a solution with the NDMA concentration of 100 mu g-L-1 in the extraction device, finally sealing the extraction device, rotating the extraction device at a rotating speed, performing vacuum filtration through a filter membrane after a certain time to obtain a water sample, and testing the NDMA concentration of the water sample through a liquid chromatograph.

Description

Water treatment method for N-nitrosodimethylamine in ferroferric oxide reinforced zero-valent iron reduction water
Technical Field
The invention relates to the field of surface water treatment, in particular to a chemical method for strengthening zero-valent iron to reduce pollutants in water.
Background
N-Nitrosodimethylamine (NDMA) is a strong carcinogenic pollutant in water, and can enter living cells and mammals through various ways such as respiratory tract inhalation, digestive tract ingestion, skin contact and the like to cause gene mutation, researchers in 1956 find that NDMA can cause poisoning and death of mice, the environmental protection agency in the United states has determined that the mass concentration corresponding to the unit carcinogenic risk is 0.7 ng L-1 and lists the NDMA as a B2 carcinogen, numerous researches find that NDMA as a byproduct is generated in the disinfection process of drinking water chlorine and chloramine, and in domestic and foreign investigation researches, NDMA with higher concentration is detected in the treatment effluent of urban drinking water, and far exceeds the highest acceptable concentration of NDMA in the drinking water, which is respectively regulated by the health service department of California and the environmental protection agency of Canada, by 10 ng L-1 and 9 ng L-1.
NDMA is a semi-volatile, readily water-soluble organic compound that, coupled with its low vapor pressure and low henry's law constant, is difficult to remove from natural bodies of water by either volatilization or stripping. The treatment techniques for this contaminant in the prior art include biological methods, adsorption methods, advanced oxidation methods, and metal reduction methods. The biological method is economical and safe, but has long reaction time, and the reaction time is up to several years; the adsorbing material can adsorb NDMA in a water body, but the adsorbing material is easy to saturate and needs to be replaced regularly, and whether the adsorbing material can be safely recycled or not is unknown; the NDMA can be quickly and efficiently removed by ultraviolet photolysis in the advanced oxidation method, but the extra energy consumption increases the treatment cost; the zero-valent iron in the metal reduction technology can reduce various chlorinated organic matters in water, and the technology is widely applied to in-situ remediation of soil and underground water in a form of a permeable reaction grid, but the removal rate of NDMA is slow, and the reaction period is long.
Disclosure of Invention
The invention aims to solve the existing problems, the ferroferric oxide is multivalent iron oxide, the physicochemical property of the ferroferric oxide is stable, the source is wide, related researches propose that the ferroferric oxide can serve as a conductor to accelerate the electron transfer between zero-valent iron and a pollution target object, in addition, the ferroferric oxide has weak magnetism, the existing researches show that the weak magnetic field can influence the charged ion distribution on the surface of the zero-valent iron, and the two conditions are both beneficial to improving the reducing capability of the zero-valent iron. Therefore, based on the possible influence of ferroferric oxide on zero-valent iron, the research applies a coexisting system of the ferroferric oxide and the zero-valent iron to the removal reaction of NDMA (ferric nitrate-dimethyl-amine) and finds a technology which has low cost and low energy consumption and can effectively control the strong carcinogenic substance Nitrosodimethylamine (NDMA) in water, thereby widening the implementation path of the application technology of safety guarantee of surface water and drinking water.
The technical scheme adopted by the invention for solving the technical problems is as follows: the water treatment method of N-nitrosodimethylamine in ferroferric oxide reinforced zero-valent iron reduction water comprises the following steps:
s1, preparing a buffer solution, and adjusting the pH value of the buffer solution, wherein the buffer solution is any one of 1, 4-piperazine dipropyl sulfonic acid and 4-hydroxyethyl piperazine ethanesulfonic acid;
s2, measuring the buffer solution in the S1, adding the buffer solution into extraction equipment, sequentially adding iron powder, ferroferric oxide and NDMA mother solution into the extraction equipment, preparing a solution with the NDMA concentration of 100 mu g-L-1 in the extraction equipment, and finally sealing the extraction equipment;
s3, rotating the extraction equipment sealed in the S2 at a rotating speed, and after a certain time, carrying out vacuum filtration on the solution in the extraction equipment through a filter membrane to obtain a water sample;
and S4, testing the NDMA concentration of the water sample subjected to suction filtration in the S3 by a liquid chromatograph.
Preferably, the buffer solution is a solution ofThe quantitative concentration is 25 mmol-L-1。
Preferably, the pH range of the buffer solution is 4-7.
Preferably, the concentration of the iron powder is 10 g. L-1。
Preferably, the concentration of the ferroferric oxide is 1.25-20 g. L-1。
Preferably, the extraction device in S3 is placed on a rotary incubator and rotated at a rotating speed.
Preferably, the rotation speed of the rotation speed is 45 r min-1。
Preferably, the rotation speed is rotated for 6, 12, 24, 72, 120 or 168 h.
Preferably, the diameter of the filter membrane is 0.22-0.45 μm.
The invention has the beneficial effects that: the research researches the removal situation of N-nitrosodimethylamine which is a strong carcinogenic substance in water when magnetic iron oxide, namely ferroferric oxide and zero-valent iron coexist. Compared with the research of catalyzing zero-valent iron by using the existing noble metal and other catalysts, the ferroferric oxide has the advantages of low price, clean materials and no secondary pollution, in addition, the special weak magnetism is simpler than that of the existing research of catalyzing zero-valent iron by using an external weak magnetic field or pre-magnetizing the zero-valent iron, the combined application operation of the zero-valent iron and the ferroferric oxide is simple, the energy consumption is low, and the development of the technology is more beneficial to the application of the zero-valent iron reduction technology to the treatment of surface water.
Drawings
FIG. 1 shows the removal of NDMA in the presence of single zero-valent iron, single ferroferric oxide and both zero-valent iron and ferroferric oxide.
FIG. 2 shows the removal of NDMA in the presence of zero-valent iron and ferroferric oxide at pH 4 and 7.
FIG. 3 shows the removal of NDMA in the presence of 10g, L-1, zero-valent iron, 10g, L-1, and 20 g, L-1, ferroferric oxide.
Detailed Description
The technical solution of the present invention is further specifically described below by way of specific examples in conjunction with the accompanying drawings.
Example 1: reagents used for the experiment: iron powder (analytically pure), 4-hydroxyethylpiperazine ethanesulfonic acid (analytically pure), ferroferric oxide (analytically pure), nitrosodimethylamine pure product (> 99%), sodium hydroxide (analytically pure)
The apparatus used in the experiment comprises a rotary incubator (QB-328), a PH meter (Raynaud magnetic PHS-3C), a high performance liquid chromatograph (Shimadzu L C-20A), a circulating water type multipurpose vacuum pump (SHB-IIIA), and an extraction device (brown extraction bottle)
The method comprises the specific experimental steps of preparing a 4-hydroxyethyl piperazine ethanesulfonic acid buffer solution (HEPES) with the mass concentration of 25 mmol, L-1, adding a prepared 1mol L-1 sodium hydroxide solution, adjusting the pH value of the solution to 7 by using a pH meter, measuring 40 m L, adding the solution into a brown extraction bottle, sequentially adding 10g L-1 of iron powder, 10g L-1 of ferroferric oxide and a certain amount of NDMA mother liquor to enable the initial concentration to be 100 mu g L-1 into the reaction bottle, tightly covering the bottle, placing the bottle on a rotary culture device to rotate at a rotating speed of 45 r.min-1, after a certain time (the sampling time of the experiment is respectively 6, 12, 24, 72, 120 and 168 hours), carrying out vacuum filtration on the reacted solution through a 0.45 mu m filter membrane, after the reaction is stopped, taking a water sample after the suction filtration, testing the concentration of NDMA through a liquid chromatograph after the reaction is finished, and repeating the experiment for three times.
Example 2: reagents used for the experiment: iron powder (analytically pure), 1, 4-piperazine dipropylsulfonic acid (analytically pure), ferroferric oxide (analytically pure), nitrosodimethylamine pure product (> 99%), sodium hydroxide (analytically pure)
The apparatus used in the experiment comprises a rotary incubator (QB-328), a PH meter (Raynaud magnetic PHS-3C), a high performance liquid chromatograph (Shimadzu L C-20A), a circulating water type multipurpose vacuum pump (SHB-IIIA), and an extraction device (brown extraction bottle)
The method comprises the specific experimental steps of preparing 1, 4-piperazine dipropylsulfonic acid buffer solution (PIPPS) with the mass concentration of 25 mmol, L-1, adding 1mol L-1 sodium hydroxide solution, adjusting the pH value of the solution to 4 by using a pH meter, measuring 40 m L, adding the solution into a brown extraction bottle, sequentially adding 10g L-1 iron powder, 10g L-1 ferroferric oxide and a certain amount of NDMA mother liquor to enable the initial concentration to be 100 mu g, L-1, tightly covering the bottle, placing the bottle on a rotary culture device to rotate at the rotating speed of 45 r.min-1, after a certain time (the sampling time of the experiment is respectively 6, 12, 24, 72, 120 and 168 hours), carrying out vacuum filtration on the reacted solution through a 0.45 mu m filter membrane, after the reaction is ended, taking a water sample after 1m L, testing the concentration of NDMA through a liquid chromatograph, and repeating the experiment for three times.
Example 3: reagents used for the experiment: iron powder (analytically pure), 4-hydroxyethylpiperazine ethanesulfonic acid (analytically pure), ferroferric oxide (analytically pure), nitrosodimethylamine pure product (> 99%), sodium hydroxide (analytically pure)
The apparatus used in the experiment comprises a rotary incubator (QB-328), a PH meter (Raynaud magnetic PHS-3C), a high performance liquid chromatograph (Shimadzu L C-20A), a circulating water type multipurpose vacuum pump (SHB-IIIA), and an extraction device (brown extraction bottle)
The method comprises the specific experimental steps of preparing a 4-hydroxyethyl piperazine ethanesulfonic acid buffer solution (HEPES) with the mass concentration of 25 mmol, L-1, adding a prepared 1mol L-1 sodium hydroxide solution, adjusting the pH value of the solution to 7 by using a pH meter, measuring 40 m L, adding the solution into a brown extraction bottle, sequentially adding 10g of L-1 iron powder, 20 g of L-1 ferroferric oxide and a certain amount of NDMA mother liquor to enable the initial concentration to be 100 mu g, L-1 into the reaction bottle, tightly covering the bottle, placing the reaction bottle on a rotary incubator to rotate at the rotating speed of 45 r.min-1, after a certain time (the sampling time of the experiment is respectively 6, 12, 24, 72, 120 and 168 hours), carrying out vacuum filtration on the reacted solution through a 0.45 mu m filter membrane, after the reaction is stopped, taking a water sample after the suction filtration, testing the concentration of NDMA through a liquid chromatograph, and repeating the experiment three times.
FIG. 1 shows the removal of NDMA in the presence of single zero-valent iron, single ferroferric oxide and both zero-valent iron and ferroferric oxide. As can be seen from the figure, the NDMA can be removed by using the single zero-valent iron, but the reaction is slow, the single ferroferric oxide does not react with the NDMA, but when the zero-valent iron and the ferroferric oxide coexist, the NDMA concentration is obviously reduced, the removal effect of the coexisting system is greater than the sum of the two, and the NDMA removal rate reaches about 80% after the system reacts for 7 days. In addition, from the view point of reaction rate, it is faster than zero-valent iron, and the later reaction is in a growing trend. From the above phenomena, it is known that ferroferric oxide can strengthen the reduction of NDMA by zero-valent iron.
FIG. 2 shows the removal of NDMA in the presence of zero-valent iron and ferroferric oxide at pH 4 and 7. As can be seen from the graph, the reaction effect of the solution pH of 4 is better than that of the solution pH of 7, the removal rate is increased by more than 5% in the same way, the reaction rate is faster, and the removal effect of NDMA is gradually increased along with the decrease of the solution pH.
FIG. 3 shows the NDMA removal situation under the coexistence of 10g, L-1 zero-valent iron and 10g, L-1 iron oxide and 20 g, L-1 ferroferric oxide, respectively, it can be seen from the figure that 20 g, L-1 iron oxide has better reaction effect than 10g, L-1 iron oxide, the removal rate is increased by more than 5% after 24h reaction, the reaction rate is faster, and the NDMA removal is positively correlated with the ferroferric oxide concentration under the coexistence system.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.

Claims (9)

1. The water treatment method for reducing N-nitrosodimethylamine in water by ferroferric oxide reinforced zero-valent iron is characterized by comprising the following steps of:
s1, preparing a buffer solution, and adjusting the pH value of the buffer solution, wherein the buffer solution is any one of 1, 4-piperazine dipropyl sulfonic acid and 4-hydroxyethyl piperazine ethanesulfonic acid;
s2, measuring the buffer solution in the S1, adding the buffer solution into extraction equipment, sequentially adding iron powder, ferroferric oxide and NDMA mother solution into the extraction equipment, preparing a solution with the NDMA concentration of 100 mu g-L-1 in the extraction equipment, and finally sealing the extraction equipment;
s3, rotating the extraction equipment sealed in the S2 at a rotating speed, and after a certain time, carrying out vacuum filtration on the solution in the extraction equipment through a filter membrane to obtain a water sample;
and S4, testing the NDMA concentration of the water sample subjected to suction filtration in the S3 by a liquid chromatograph.
2. The method for treating N-nitrosodimethylamine in ferroferric oxide-enhanced zero-valent iron reduced water according to claim 1, wherein the mass concentration of the buffer solution is 25 mmol-L-1。
3. The method for treating N-nitrosodimethylamine in ferroferric oxide-enhanced zero-valent iron reduced water according to claim 1, wherein the pH of the buffer solution is 4-7.
4. The method for treating N-nitrosodimethylamine in ferroferric oxide-strengthened zero-valent iron reduced water according to claim 1, wherein the concentration of said iron powder is 10 g-L-1。
5. The method for treating N-nitrosodimethylamine in ferroferric oxide reinforced zero-valent iron reduced water according to claim 1, wherein the concentration of the ferroferric oxide is 1.25-20 g-L-1。
6. The method for treating N-nitrosodimethylamine in ferroferric oxide-enhanced zero-valent iron reduced water according to claim 1, wherein the extraction equipment in S3 is placed on a rotary incubator and rotated at a rotating speed.
7. The method for treating N-nitrosodimethylamine in ferroferric oxide-enhanced zero-valent iron reduced water according to claim 6, wherein the rotating speed is 45 r-min-1。
8. The method for treating N-nitrosodimethylamine in ferroferric oxide reinforced zero-valent iron reduced water according to claim 1, wherein the time of the rotation at the rotating speed is 6, 12, 24, 72, 120 or 168 hours.
9. The method for treating N-nitrosodimethylamine in ferroferric oxide reinforced zero-valent iron reduced water according to claim 1, wherein the diameter of the filter membrane is 0.22-0.45 μm.
CN202010131012.3A 2020-02-28 2020-02-28 Water treatment method for N-nitrosodimethylamine in ferroferric oxide reinforced zero-valent iron reduction water Pending CN111453875A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113307349A (en) * 2021-04-21 2021-08-27 中科院广州化学有限公司 NDMA (non-catalytic oxidative degradation) degradation method based on graphene/iron-based MOF (metal organic framework) composite nanomaterial and application

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101306862A (en) * 2008-07-01 2008-11-19 浙江大学 Method for preparing nano-level Fe<0>/Fe3O4 and uses thereof
CN102884010A (en) * 2009-09-18 2013-01-16 得克萨斯州A&M大学系统 Zero valent iron/iron oxide mineral/ferrous iron composite for treatment of a contaminated fluid
CN105645551A (en) * 2015-12-31 2016-06-08 浙江工业大学 Treatment method for reducing nitrosodimethylamine in water by catalyzing zero-valent iron through copper corrosion product
US20180305229A1 (en) * 2015-10-21 2018-10-25 The Texas A&M University System Method for removal of recalcitrant selenium species from wastewater
CN110357240A (en) * 2019-05-15 2019-10-22 浙江工业大学 Patina cooperates with the method for treating water of nitrosodimethylamine in Zero-valent Iron reductive water

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101306862A (en) * 2008-07-01 2008-11-19 浙江大学 Method for preparing nano-level Fe<0>/Fe3O4 and uses thereof
CN102884010A (en) * 2009-09-18 2013-01-16 得克萨斯州A&M大学系统 Zero valent iron/iron oxide mineral/ferrous iron composite for treatment of a contaminated fluid
US20180305229A1 (en) * 2015-10-21 2018-10-25 The Texas A&M University System Method for removal of recalcitrant selenium species from wastewater
CN105645551A (en) * 2015-12-31 2016-06-08 浙江工业大学 Treatment method for reducing nitrosodimethylamine in water by catalyzing zero-valent iron through copper corrosion product
CN110357240A (en) * 2019-05-15 2019-10-22 浙江工业大学 Patina cooperates with the method for treating water of nitrosodimethylamine in Zero-valent Iron reductive water

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113307349A (en) * 2021-04-21 2021-08-27 中科院广州化学有限公司 NDMA (non-catalytic oxidative degradation) degradation method based on graphene/iron-based MOF (metal organic framework) composite nanomaterial and application

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