CN107055893B - Method for treating wastewater containing low-concentration DMF - Google Patents

Method for treating wastewater containing low-concentration DMF Download PDF

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CN107055893B
CN107055893B CN201710291677.9A CN201710291677A CN107055893B CN 107055893 B CN107055893 B CN 107055893B CN 201710291677 A CN201710291677 A CN 201710291677A CN 107055893 B CN107055893 B CN 107055893B
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dmf
waste water
oxidant
wastewater
treatment solution
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CN107055893A (en
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张晓亮
吴小亮
吴勇前
王仁醒
陶海祥
楼银川
吕杨
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Zhejiang Qi Cai Eco Technology Co ltd
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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
    • C02F1/30—Treatment of water, waste water, or sewage by irradiation
    • C02F1/302—Treatment of water, waste water, or sewage by irradiation with microwaves
    • 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
    • C02F1/30—Treatment of water, waste water, or sewage by irradiation
    • C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
    • 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
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • 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
    • C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • 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
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
    • 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
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2301/00—General aspects of water treatment
    • C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions

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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)
  • Treatment Of Water By Oxidation Or Reduction (AREA)
  • Physical Water Treatments (AREA)

Abstract

The invention discloses a method for treating wastewater containing low-concentration DMF, which comprises the following steps: (1) acid hydrolysis: adding a soluble metal salt catalyst into DMF wastewater, adjusting the pH to 1-5, and carrying out acidolysis treatment, wherein the catalytic acidolysis time is 20-120min, and the acidolysis temperature is 40-60 ℃, so as to obtain a treatment solution 1; (2) and (3) oxidation reaction: adding an oxidant into the treatment solution 1, and carrying out oxidation reaction in microwave equipment for 5-180min to obtain a treatment solution 2; (3) photocatalytic oxidation: adjusting the pH value of the treatment liquid 2 to 6-9, flocculating and filtering, and finally adding an oxidant and a catalyst for photocatalytic oxidation for 30-120 min. The method can reduce COD and TOC in the wastewater while removing DMF, greatly improve the mineralization degree and the biochemical property of the wastewater, and has the advantages of simple process flow, mild reaction condition, simple operation, obvious effect and better economic benefit.

Description

Method for treating wastewater containing low-concentration DMF
Technical Field
The invention relates to the technical field of industrial wastewater, in particular to a method for treating wastewater containing low-concentration DMF (dimethyl formamide).
Background
N, N-Dimethylformamide (DMF) is an important chemical raw material and an organic solvent, is stable in property, is difficult to biodegrade (B/C is 0.065), and has certain toxicity. The method is widely applied to the fields of pesticides, medicines, polyurethane synthetic leather, butadiene extraction, dye solvents, dye synthetic raw materials and the like. At present, DMF wastewater treatment processes can be roughly divided into two categories, namely a DMF recovery process (suitable for high-concentration DMF wastewater of more than 10%) and a degradation removal process (suitable for low-concentration DMF) which take rectification as a core; wherein the degradation technology can be divided into biochemical technology and physical and chemical degradation technology (alkaline hydrolysis, acidolysis and oxidation) and the like, and is mainly suitable for treating low-concentration DMF wastewater.
DMF has a high boiling point (153 ℃), and energy consumption is huge when rectification recovery is adopted, so that the method is only suitable for recovery treatment of high-concentration DMF, and the method is generally considered in industry when the DMF content is more than 10%. For example, patent CN201510092727 relates to a DMF wastewater treatment device and method, wherein the concentration of DMF recovered by rectification is 10-80%. Patent CN201510724317 is a waste water treatment system for low-cost DMF recovery, and the concentration of DMF in DMF recovery waste water is 15-20%.
The solvent extraction method is also suitable for waste water with high DMF concentration, but has strict requirements on the selection conditions of an extracting agent and the problem of secondary pollution of the solvent.
The activated carbon adsorption method is only suitable for low-concentration DMF wastewater, the activated carbon can be frequently regenerated under high concentration, and the adsorbent is large in dosage and is not suitable for large-scale industrial production.
DMF is decomposed into dimethylamine and formate under the action of alkali, dimethylamine is volatile, and dimethylamine can be taken out in an air stripping or steam stripping mode so as to achieve the purpose of reducing COD (chemical oxygen demand) of DMF wastewater.
The DMF waste water biochemical method mainly comprises an activated sludge method and a high-efficiency strain biological strengthening method. However, the biodegradability of DMF is poor (B/C is 0.065), the treatment effect is not ideal, the requirement of yielding water is difficult to achieve, and the tolerance to the entering water DMF is low. The biochemical treatment in the method for treating organic nitrogen DMF chemical wastewater in patent CN20151072525.1 requires that the total nitrogen of inlet water is less than or equal to 200mg/L (DMF is about 1000 ppm).
Patent "a pretreatment method of waste water containing low concentration of N, N-dimethylformamide" CN201410546709 reports a method of acid hydrolysis of DMF under the action of aluminum trichloride, zinc chloride, magnesium chloride, etc., wherein the DMF concentration is 6000ppm, the pH is less than 2, 0.2% of aluminum trichloride is added, and the reaction is carried out at 50 ℃ for 50min, and the DMF concentration is reduced to 23 ppm. The patent only makes DMF hydrolyze under acidity, and the products of DMF acidolysis are formic acid and dimethylamine salt, although the concentration of DMF is reduced, COD and TOC of the wastewater are not removed.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for treating wastewater containing low-concentration DMF (dimethyl formamide), which can reduce COD (chemical oxygen demand) and TOC (total organic carbon) in the wastewater and greatly improve the mineralization degree and biodegradability of the wastewater while removing DMF.
A method for treating waste water containing low-concentration DMF is characterized by comprising the following steps:
(1) acid hydrolysis: adding a soluble metal salt catalyst into DMF wastewater, adjusting the pH value to 1-5, and carrying out acidolysis treatment, wherein the catalytic acidolysis time is 20-120min, and the acidolysis temperature is 40-70 ℃, so as to obtain a treatment solution 1;
(2) and (3) oxidation reaction: adding an oxidant into the treatment solution 1, and carrying out oxidation reaction for 5-180min to obtain a treatment solution 2;
(3) photocatalytic oxidation: and adding a flocculating agent into the treatment liquid 2, adjusting the pH value to 6-9, flocculating and filtering, and finally adding an oxidant for ultraviolet light oxidation for 30-120 min.
The low-concentration DMF wastewater of the invention refers to wastewater with the mass volume concentration of DMF less than 30000 mg/L.
Preferably, the soluble metal salt catalyst in the step (1) is one or a mixture of more of soluble iron, copper, zinc, nickel and manganese salts, and the adding amount of the catalyst is 0.01-0.5% of the mass of the wastewater. More preferably, the soluble metal salt catalyst is one or more of ferrous sulfate, ferrous chloride, ferric sulfate, ferric chloride, copper sulfate, copper chloride, copper nitrate, zinc chloride, zinc sulfate, zinc nitrate, nickel chloride, nickel sulfate, nickel nitrate, manganese sulfate, manganese chloride and manganese nitrate.
Preferably, in the step (1), the pH value of the DMF wastewater is adjusted to 1-3.
And (3) in the step (2), the oxidant is one or more of hydrogen peroxide, sodium hypochlorite, peroxymonosulfate and peroxydisulfate, and the adding amount of the oxidant is 2-35 times of the content of DMF in the treatment solution 1. When the oxidant is hydrogen peroxide, the adding amount of the hydrogen peroxide is 5-15 times of the content of DMF in the treating fluid 1, wherein the adopted hydrogen peroxide is a commercially available finished product.
Preferably, the step (2) can be carried out in a microwave radiation environment, the oxidation reaction time is 10-60 min, and the microwave power required by every 1000g of wastewater is 50-5000W, preferably 500-2000W. Wherein, the microwave frequency can be 2450MHz or 915 MHz.
More preferably, the microwave irradiation in step (2) is performed in the environmentAdding a sensitizer, wherein the sensitizer is activated carbon and Fe3O4、CuO、Ni2O3、MnO2、CoO4、CdO、V2O5One or more of SiC and chromium slag, wherein the adding amount of the sensitizer is 0.05-5% of the mass of the DMF wastewater by mass. Further preferably, the sensitizer is activated carbon.
And (3) adding a flocculating agent in the flocculation process in the step (3), wherein the flocculating agent can be one or more of Polyacrylamide (PAM), chitosan, polyferric chloride and polyaluminium chloride, and the adding amount of the flocculating agent is 0.0001-0.1% of the mass of the wastewater.
The pH of the treatment liquid 2 may be adjusted by using an alkaline substance in the step (3). Preferably, NaOH, CaO, Ca (OH) can be used in step (3)2、Na2CO3And one or more of liquid alkali and ammonia water are used for adjusting the pH value of the treatment liquid 2.
Further preferably, the pH value of the photooxidation reaction in the step (3) is 6-9.
And (3) the oxidant is one or more of hydrogen peroxide, peroxymonosulfate and peroxydisulfate, and the adding amount of the oxidant is 1-8% of the mass of the treatment solution 2.
The method treats the waste water containing DMF with lower concentration, the DMF is hydrolyzed under the acidic condition, and the products generated by the acidolysis are formic acid and dimethylamine salt; the subsequent oxidation reaction has one less intermediate process than the direct oxidation of DMF, so that the oxidant has high utilization rate and is easy to oxidize into small molecular organic matter; small molecular organic matters, formate and the like are further oxidized by ultraviolet light. The method can effectively reduce COD and TOC in the wastewater while removing DMF, and greatly improve the mineralization degree and biodegradability of the wastewater. The method has the advantages of simple process flow, mild reaction conditions, simple operation, obvious effect and better economic benefit.
Detailed Description
Example 1
N, N-Dimethylformamide (DMF) wastewater with a concentration of 5000mg/L and a TOC of 2384 mg/L.
(1) Taking 300mL of DMF wastewater, and adjusting the pH value to be the same with concentrated hydrochloric acid2.0, adding 0.3g of ZnSO in sequence4·7H2O、0.9gFeSO4·7H2O), and stirring and reacting for 30min at 60 ℃ to obtain a treatment solution 1.
(2) Adding 15g of hydrogen peroxide (27 wt%) and 0.3g of powdered activated carbon into the treatment liquid 1 obtained in the step (1), placing the treatment liquid in a microwave device, starting mechanical stirring simultaneously, and carrying out microwave synergistic oxidation treatment for 60min to obtain a treatment liquid 2, wherein the microwave power is 200W.
To the resulting treatment liquid 2, 0.009g of chitosan and 0.015g of PAM were added, stirred for 5min, then adjusted to pH 8 with liquid alkali (30 wt%), left to stand for 20min and filtered.
Through measurement, the concentration of DMF in the treatment solution 2 is reduced to 115mg/L, the removal rate is 97.7 percent, the TOC is reduced to 620mg/L, and the removal rate is 74 percent.
(3) And (3) carrying out photooxidation on the treatment liquid 2 for 60min to obtain a treatment liquid 3, wherein the feeding amount of DMF wastewater is 250g, the pH value of the wastewater is 8, the ultraviolet power is 500W, and the using amount of hydrogen peroxide (27 wt%) is 5 g.
Through measurement, the concentration of DMF in the treatment solution 3 is reduced to 8mg/L, the removal rate is 99.8 percent, the TOC is reduced to 310mg/L, and the removal rate is 87 percent.
Example 2
N, N-Dimethylformamide (DMF) wastewater at a concentration of about 16550mg/L and a TOC of 7877 mg/L.
(1) Taking 100mL of DMF wastewater, adjusting the pH value to 2.0 by using concentrated sulfuric acid, and sequentially adding 0.3g of ZnSO4·7H2O、0.5gFeSO4·7H2And O, stirring and reacting for 60min at the temperature of 60 ℃ to obtain a treatment solution 1.
(2) And (2) adding 10g of potassium hydrogen peroxymonosulfate and 0.1g of powdered activated carbon into the treatment liquid 1 obtained in the step (1), placing the treatment liquid in a microwave device, starting mechanical stirring at the same time, and carrying out microwave synergistic oxidation treatment for 60min to obtain a treatment liquid 2. Wherein the microwave power is 200W.
To the resulting treated liquid 2 were added 0.005g of chitosan and 0.08g of PAC, and after stirring for 5min, the pH was adjusted to 8 with liquid alkali (30 wt%), and the mixture was left to stand for 20min and filtered.
Through determination, the concentration of DMF in the treatment solution 2 is reduced to 993mg/L, the removal rate is 94%, the TOC is reduced to 2442mg/L, and the removal rate is 69%.
Example 3
The same DMF waste water as in example 2 was used for the treatment.
(1) Taking 100mL of DMF wastewater, adjusting the pH value to 2.0 by using concentrated hydrochloric acid, and sequentially adding 0.2g of ZnSO4·7H2O、0.4gFeSO4·7H2O, stirring at 60 ℃ for 60min to obtain a treatment solution 1.
(2) Adding 8g of hydrogen peroxide (27 wt%) into the treatment solution 1 obtained in the step (1), and continuously reacting for 2 hours to obtain a treatment solution 2. To the resulting treatment liquid 2, 0.05g of chitosan and 0.08g of PAC were added, stirred for 5min, added dropwise with liquid caustic soda (30 wt%), adjusted to pH 8, left to stand for 20min, and filtered.
The DMF concentration of the treatment solution 2 was reduced to 780mg/L, the removal rate was 95%, the TOC was reduced to 3072mg/L, and the removal rate was 61%.
Comparative example 1
The same DMF waste water as in example 1 was used for the treatment. The conditions were unchanged compared to example 1 except that in step (3) the photooxidation pH was 3.
As a result: the DMF concentration of the treatment solution (3) was reduced to 73mg/L, the removal rate was 98.54%, the TOC was reduced to 453mg/L, and the removal rate was 81%.
Comparative example 2
The same DMF waste water as in example 2 was used for the treatment. Taking 100mL of DMF waste water, adjusting the pH value to 1.6 by concentrated hydrochloric acid, adding 33.16mg (2 percent of DMF content in the waste water) of magnesium chloride, heating to 60 ℃, and stirring for reaction for 180 min. The concentration of DMF was determined to be 15500mg/L and the TOC was determined to be 7580 mg/L.
Comparative example 3
The same DMF waste water as in example 3 was used for the treatment. In comparison with example 3, step (1) did not add ZnSO4·7H2O, the retention time is 0min, and the rest conditions are unchanged.
As a result: the concentration of DMF in the treatment solution (2) is reduced to 3806.5mg/L, and the removal rate is 77 percent; TOC was reduced to 5277.6mg/L with a removal rate of 33%.
Comparative example 4
The same DMF waste water as in example 3 was used for the treatment. Compared with example 3Addition of ZnSO in the step (1)4·7H2Except O, the other conditions were unchanged.
As a result: the concentration of DMF in the treatment solution (2) is reduced to 2813mg/L, and the removal rate is 83 percent; TOC was reduced to 4017mg/L with a removal rate of 49%.

Claims (6)

1. A method for treating waste water containing low-concentration DMF is characterized by comprising the following steps:
(1) acid hydrolysis: adding a soluble metal salt catalyst into DMF wastewater, adjusting the pH value to 1-5, and carrying out acidolysis treatment for 20-120min at the acidolysis temperature of 40-70 ℃ to obtain a treatment solution 1; the soluble metal salt catalyst is one or a mixture of more of soluble iron, copper, zinc, nickel and manganese salts, and the adding amount of the catalyst is 0.01-0.5% of the mass of the wastewater;
(2) and (3) oxidation reaction: adding an oxidant into the treatment solution 1, and carrying out oxidation reaction for 5-180min to obtain a treatment solution 2; the oxidant is one or more of hydrogen peroxide, sodium hypochlorite, peroxymonosulfate and peroxydisulfate, and the adding amount of the oxidant is 2-35 times of the content of DMF in the treatment solution 1;
(3) photocatalytic oxidation: adding a flocculating agent into the treatment liquid 2, adjusting the pH value to 6-9, flocculating and filtering, and finally adding an oxidant for ultraviolet catalytic oxidation for 30-120 min; the oxidant is one or more of hydrogen peroxide, peroxymonosulfate and peroxydisulfate, and the adding amount of the oxidant is 1-8% of the mass of the treatment solution 2.
2. The method for treating wastewater containing low-concentration DMF according to claim 1, characterized in that the oxidant in the step (2) is hydrogen peroxide, and the adding amount of the hydrogen peroxide is 5-15 times of the content of DMF in the treating fluid 1.
3. The method for treating waste water containing low concentration of DMF according to claim 1, wherein the oxidation reaction in step (2) is carried out in a microwave irradiation environment, the microwave power required for each 1000g of waste water is 50-5000W, and a sensitizer is added into the waste water.
4. The method for treating waste water containing low concentration of DMF as claimed in claim 3, wherein the microwave power is 500-2000W per 1000g of waste water.
5. The method for treating waste water containing low concentration of DMF according to claim 1, characterized in that flocculating agent is added in the flocculation process of step (3), the flocculating agent is one or more of polyacrylamide, chitosan, polymeric ferric chloride and polymeric aluminum chloride, and the adding amount of the flocculating agent is 0.0001-0.1% of the mass of the waste water.
6. The method for treating waste water containing low concentration of DMF as claimed in claim 1, wherein step (3) employs NaOH, CaO, Ca (OH)2、Na2CO3And one or more of ammonia water to adjust the pH value of the treatment liquid 2.
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CN108640406A (en) * 2018-03-28 2018-10-12 广西金茂生物化工有限公司 A method of utilizing microwave treatment cassava alcohol waste water
CN108862717B (en) * 2018-07-06 2021-08-24 山东潍坊润丰化工股份有限公司 Resourceful treatment method of low-concentration amide wastewater
CN111054203B (en) * 2019-12-30 2023-12-22 陕西鼓风机（集团）有限公司 Tail gas treatment method and system for DMF wastewater
CN112279407A (en) * 2020-10-20 2021-01-29 山东潍坊润丰化工股份有限公司 Method for treating dimethylamine wastewater
CN114811624A (en) * 2021-01-22 2022-07-29 中国科学院大学 DMF-containing waste gas purification and collaborative production N 2 Method of O
CN113562894B (en) * 2021-08-20 2023-05-09 桂林南药股份有限公司 DMF wastewater and DMSO wastewater treatment method and treatment system
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CN115072903B (en) * 2022-07-12 2024-01-26 安徽浩悦生态科技有限责任公司 Method for treating citric acid organic amine washing waste liquid containing N, N-dimethylformamide by using transition metal dead catalyst

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