CN107954570A - A kind of 2,5- dichloronitrobenzenes waste water treatment process - Google Patents

A kind of 2,5- dichloronitrobenzenes waste water treatment process Download PDF

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Publication number
CN107954570A
CN107954570A CN201711178435.5A CN201711178435A CN107954570A CN 107954570 A CN107954570 A CN 107954570A CN 201711178435 A CN201711178435 A CN 201711178435A CN 107954570 A CN107954570 A CN 107954570A
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CN
China
Prior art keywords
water
dichloronitrobenzenes
waste water
wastewater treatment
stripping
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201711178435.5A
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Chinese (zh)
Inventor
杨树斌
徐林
丁克鸿
沈杰
徐志斌
胡洋洋
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
NINGXIA RUITAI TECHNOLOGY Co Ltd
Jiangsu Ruixiang Chemical Co Ltd
Jiangsu Yangnong Chemical Group Co Ltd
Original Assignee
NINGXIA RUITAI TECHNOLOGY Co Ltd
Jiangsu Ruixiang Chemical Co Ltd
Jiangsu Yangnong Chemical Group Co Ltd
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Application filed by NINGXIA RUITAI TECHNOLOGY Co Ltd, Jiangsu Ruixiang Chemical Co Ltd, Jiangsu Yangnong Chemical Group Co Ltd filed Critical NINGXIA RUITAI TECHNOLOGY Co Ltd
Priority to CN201711178435.5A priority Critical patent/CN107954570A/en
Publication of CN107954570A publication Critical patent/CN107954570A/en
Pending legal-status Critical Current

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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
    • C02F1/02—Treatment of water, waste water, or sewage by heating
    • C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • C02F1/10—Treatment of water, waste water, or sewage by heating by distillation or evaporation by direct contact with a particulate solid or with a fluid, as a heat transfer medium
    • 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
    • C02F1/722—Oxidation by peroxides
    • 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
    • C02F2101/36—Organic compounds containing halogen
    • 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
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00—Biological treatment of water, waste water, or sewage
    • C02F3/02—Aerobic processes
    • C02F3/12—Activated sludge processes
    • C02F3/1236—Particular type of activated sludge installations
    • C02F3/1263—Sequencing batch reactors [SBR]

Abstract

The present invention relates to a kind of waste water treatment process, and in particular to a kind of 2,5 dichloronitrobenzene waste water treatment process, belong to Fine Chemistry Wastewater processing technology field.The present invention includes the following steps：The first step, 2,5 dichloronitrobenzene waste water enter stripper after preheating, and stripping discharging enters oil-water decanter, and water layer returns to stripping tower reactor, oil reservoir recycling, and stripping vessel water enters next process；Second step, stripping vessel water cooling, adds acid for adjusting pH, then adds a certain amount of hydrogen peroxide and be uniformly mixed；3rd step, will mix the waste water of hydrogen peroxide, controls certain temperature and flow velocity, into the fixed bed reactors of loading catalyst, carry out catalytic oxidation；4th step, after oxidation water outlet neutralizes, into biochemistry pool, the qualified discharge after biochemical treatment.Solve the discharge problem of existing waste water, during produced without the secondary pollution such as iron cement solid waste, there is operating condition gentle, flexible operation mode, treatment effect is reliable and stable, is easy to industrializing implementation, with very broad prospect of application.

Description

A kind of 2,5- dichloronitrobenzenes waste water treatment process
Technical field
The present invention relates to a kind of waste water treatment process, and in particular to one kind 2,5- dichloronitrobenzene waste water treatment process, belongs to In Fine Chemistry Wastewater processing technology field.
Background technology
2,5- dichloronitrobenzenes are important chemical intermediates, are widely used in the industries such as pesticide, dyestuff.The country 2 at present, The production of 5- dichloronitrobenzenes mainly uses paracide mixed acid nitrification, is separated through oleic acid, alkali cleaning, washing, rectifying obtain product, During produce a large amount of waste water, paracide, 2,5- dichloronitrobenzenes, phenates class (such as nitro diclophenac sodium, dinitro are contained in waste water Base diclophenac sodium etc.) etc., there is COD concentration height, difficult for biological degradation, environmental pollution is serious.
On 2,5- dichloronitrobenzene wastewater treatments, Chinese patent CN101597116A mentions one kind 2,5- dichloronitrobenzenes Waste water treatment process, using modes such as catalysis and micro-electrolysis, catalysis oxidation, activated carbon adsorptions, reduce the colourity of waste water, COD and Characteristic contamination content, realizes discharged wastewater met the national standard, but process is more, in addition can be produced during light electrolysis and Fenton oxidation Raw difficult iron cement causes secondary pollution.
The content of the invention
In order to overcome the shortcomings of in the prior art, the present invention is intended to provide one kind 2,5- dichloronitrobenzenes wastewater treatment side Method, solves the discharge problem of existing waste water, during produced without the secondary pollution such as iron cement solid waste, have that operating condition is gentle, behaviour Make that mode is flexible, treatment effect is reliable and stable, is easy to the advantages that industrializing implementation, there is very broad prospect of application.
The main water quality characteristic of 2,5- dichloronitrobenzenes raw water of the present invention is：PH value 10-14, COD 2000- 3000ppm, BOD550-150ppm, paracide 0-30ppm, 2,5- dichloronitrobenzene 100-300ppm, phenates class 300- 400ppm, NH3-N 20-80ppm。
To achieve these goals, one kind 2,5- dichloronitrobenzene waste water treatment process of the invention, using " stripping+urge The technical solution of change oxidation+biochemistry ", it is characterised in that including the following steps：
The first step, 2,5- dichloronitrobenzene waste water enter stripper after preheating, and stripping discharging enters oil-water decanter, Water layer returns to stripping tower reactor, oil reservoir recycling, and stripping vessel water enters next process；
Second step, stripping vessel water cooling, adds acid for adjusting pH, then adds a certain amount of hydrogen peroxide and be uniformly mixed；
3rd step, will mix the waste water of hydrogen peroxide, control certain temperature and flow velocity, the fixed bed into loading catalyst anti- Device is answered, carries out catalytic oxidation；
4th step, after oxidation water outlet neutralizes, into biochemistry pool, the qualified discharge after biochemical treatment.
Based on the above technical solutions, stripping process described in the first step, the kettle temperature control of stripping tower reactor is 90-110 DEG C, stripping number of plates 5-30.
Based on the above technical solutions, stripping process described in the first step, stripping discharging account for inventory ratio 5- 15%.
Based on the above technical solutions, process for preparation described in second step, is adjusted using sulfuric acid, hydrochloric acid, nitric acid etc. PH, preferably sulfuric acid.
Based on the above technical solutions, process for preparation described in second step, preferably pH adjustable range 2-7, pH scopes 3-6。
Based on the above technical solutions, process for preparation described in second step, 27.5% dioxygen water consumption 2.0g/L- 30.0g/L, preferably 5.0g/L-20.0g/L.
Based on the above technical solutions, catalytic oxidation process described in the 3rd step, controls 30-90 DEG C of temperature range, It is preferred that 50-80 DEG C.
Based on the above technical solutions, catalytic oxidation process described in the 3rd step, controls waste water certain flow rate so that In fixed bed reactors residence time 0.5-5h, preferably 0.5-3h.
Based on the above technical solutions, catalytic oxidation process described in the 3rd step, catalyst are with spherical point of ZSM-5 Son sieve is carrier, metal oxide-loaded, and metal oxide is the mixture of cupric oxide, nickel oxide and neodymia.
Based on the above technical solutions, catalytic oxidation process described in the 3rd step, metal oxide matter in catalyst Amount fraction is cupric oxide 50-70%, nickel oxide 20-40% and neodymia 5-20%.
Based on the above technical solutions, biochemical treatment process described in the 4th step, adds alkali to adjust oxidation water outlet pH models Enclose 7-9.
The present invention has the following advantages that compared with prior art：
1. by separating and recovering paracide and 2,5- dichloronitrobenzene in waste water, characteristic contamination concentration and processing are reduced Difficulty, improves treatment effect, reduces processing cost.
2. using fixed bed reactors mode, fill metal oxide-loaded catalyst and carry out catalytic oxidation, with Traditional Fenton oxidation is compared, and avoids the generation of the secondary pollution such as iron cement solid waste.
3. technological process is simple, operating condition is gentle, and water outlet after treatment meets qualified discharge.
Brief description of the drawings
Fig. 1 is 2,5- dichloronitrobenzene wastewater treatment processes.
Embodiment
Embodiment 1
Company's workshop 2,5- dichloronitrobenzene raw water features are as follows, COD 2080ppm, BOD5110ppm, pH are about 11, paracide 25ppm, 2,5- dichloronitrobenzene 223ppm, total sodium phenolate 315ppm, NH3-N40ppm。
(1) strip
2,5- dichloronitrobenzene waste water enter stripper after preheating, micro- negative in 95-105 DEG C of stripper operating temperature Pressure -0.03Mpa, under conditions of 15 pieces of theoretical cam curve, stripping discharging enters oil-water decanter, water layer overflow return stripper Kettle, oil reservoir recycling, stripping tower top discharge are stripping tower reactor water outlet COD 1250ppm, BOD under the conditions of tower amount 8.0%5 115ppm, pH about 11, paracide does not detect, 2,5- dichloronitrobenzene 12ppm, total sodium phenolate 322ppm.
(2) prepare
Following stripping vessel water is cooled to 40-80 DEG C, and 98% industrial sulphuric acid is added dropwise and adjusts pH=3-3.5, adds 27.5% Hydrogen peroxide so that 27.5% hydrogen peroxide concentration reaches 10g/L waste water, and waste water enters next process after preparation.
(3) catalysis oxidation
The preparation process of catalyst is as follows, prepares 1.0% solution with by acetic acid neodymium and deionized water first, then adds molten The spherical ZSM-5 molecular sieve of liquid weight 15%, is stirred 1h, is further dried under the conditions of 80 DEG C of drying box, then 400 DEG C calcining 10h, obtain catalyst precursor.
The catalyst precursor is immersed in the aqueous solution containing 10% copper acetate and 5% nickel acetate, 4h is stirred, into one Step is dried under the conditions of 80 DEG C of drying box, is then calcined 6h at 500 DEG C, is obtained the catalysis using spherical ZSM-5 molecular sieve as carrier Agent, catalyst metal oxide mass percent accounting cupric oxide are 60%, nickel oxide 30%, neodymia 10%.
The waste water of hydrogen peroxide will be mixed, be pumped into the tubular reactor of solid-carried catalyst, 50-60 DEG C of controlling reaction temperature, gives up Water enters next process in tubular reactor residence time 2h, water outlet.
(4) neutralize biochemical
30%NaOH solution, which is added, by catalytic oxidation treatment water outlet adjusts pH to 7.5, COD 368ppm after waste water neutralizes, BOD5205ppm, 2,5- dichloronitrobenzenes do not detect, total sodium phenolate 0.8ppm, NH3-N 45ppm。
SBR aeration tanks are directly entered by neutralizing rear oxidation water outlet, COD 95ppm, BOD after biochemical treatment 27ppm, NH3- N 12ppm, pH7.0 meet two class discharge standards.
Example 2,3, which changes, prepares material pH value in example 1, adjust pH=4-4.5, pH5-5.5, mistake with 98% sulfuric acid respectively Dioxygen water consumption, reaction temperature and residence time remain unchanged in journey, and oxidation water outlet data are as shown in table 1.
Example 4,5,6, which changes, adjusts dioxygen water consumption in example 3, be adjusted to 8g/L respectively, pH during 12g/L, 15g/L Value, reaction temperature and residence time remain unchanged, and oxidation water outlet data are as shown in table 1.
Example 7,8 changes catalysis oxidation feeding temperature in example 3, is adjusted to 60-70 DEG C respectively, 70-80 DEG C, during pH Value, dioxygen water consumption and residence time remain unchanged, and it is as shown in table 1 to aoxidize out water analysis data.
Example 9,10 changes in example 3 that waste water is in the tubular reactor residence time, 0.5h, 3h, during pH value, hydrogen peroxide Dosage and reaction temperature remain unchanged, and oxidation water outlet data are as shown in table 1.

Claims (10)

1. one kind 2,5- dichloronitrobenzene wastewater treatment methods, it is characterised in that including the following steps：
The first step, 2,5- dichloronitrobenzene waste water enter stripper after preheating, and stripping discharging enters oil-water decanter, water layer Stripping tower reactor, oil reservoir recycling are returned to, stripping vessel water enters next process；
Second step, stripping vessel water cooling, adds acid for adjusting pH, then adds a certain amount of hydrogen peroxide and be uniformly mixed；
3rd step, will mix the waste water of hydrogen peroxide, certain temperature and flow velocity is controlled, into the fixed bed reaction of loading catalyst Device, carries out catalytic oxidation；
4th step, after oxidation water outlet neutralizes, into biochemistry pool, the qualified discharge after biochemical treatment.
2. 2,5- dichloronitrobenzenes wastewater treatment method according to claim 1, it is characterised in that vapour described in the first step Process is put forward, the control of stripper kettle temperature is 90-110 DEG C, stripping number of plates 5-30.
3. 2,5- dichloronitrobenzenes wastewater treatment method according to claim 1, it is characterised in that vapour described in the first step Process is put forward, stripping discharging accounts for inventory ratio 5-15%.
4. 2,5- dichloronitrobenzenes wastewater treatment method according to claim 1, it is characterised in that match somebody with somebody described in second step Process processed, pH, preferably sulfuric acid, preferably pH adjustable range 2-7, pH scopes 3-6 are adjusted using sulfuric acid, hydrochloric acid, nitric acid etc..
5. 2,5- dichloronitrobenzenes wastewater treatment method according to claim 1, it is characterised in that match somebody with somebody described in second step Process processed, 27.5% dioxygen water consumption 2.0g/L-30.0g/L, preferably 5.0g/L-20.0g/L.
6. 2,5- dichloronitrobenzenes wastewater treatment method according to claim 1, it is characterised in that urged described in the 3rd step Change oxidizing process, 30-90 DEG C of temperature range of control, preferably 50-80 DEG C.
7. 2,5- dichloronitrobenzenes wastewater treatment method according to claim 1, it is characterised in that control one constant current of waste water Speed so that in fixed bed reactors residence time 0.5-5h, preferably 0.5-3h.
8. 2,5- dichloronitrobenzenes wastewater treatment method according to claim 1, it is characterised in that urged described in the 3rd step Change oxidizing process, catalyst be with ZSM-5 global moleculars sieve for carrier, it is metal oxide-loaded, metal oxide for cupric oxide, The mixture of nickel oxide and neodymia.
9. 2,5- dichloronitrobenzenes wastewater treatment method according to claim 1, it is characterised in that urged described in the 3rd step Change oxidizing process, metal oxide mass fraction is cupric oxide 50-70%, nickel oxide 20-40% and neodymia 5- in catalyst 20%.
10. 2,5- dichloronitrobenzenes wastewater treatment method according to claim 1, it is characterised in that described in the 4th step Biochemical treatment process, adds alkali to adjust oxidation water outlet pH scopes 7-9.
CN201711178435.5A 2017-11-23 2017-11-23 A kind of 2,5- dichloronitrobenzenes waste water treatment process Pending CN107954570A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108706772A (en) * 2018-06-08 2018-10-26 昆明理工大学 A kind of continuous treatment process of the waste water containing xanthate
CN115594357A (en) * 2022-11-08 2023-01-13 煤炭科学技术研究院有限公司（Cn） Acylation wastewater grading treatment method

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102417263A (en) * 2010-09-28 2012-04-18 中国石油化工股份有限公司 Method for processing wastewater from nitrochlorobenzene production
CN102417265A (en) * 2010-09-28 2012-04-18 中国石油化工股份有限公司 Method for effectively removing organic matters in wastewater from nitrochlorobenzene production
CN104923229A (en) * 2014-03-21 2015-09-23 中国科学院大连化学物理研究所 Activated carbon catalyst used for Fenton-like technology, and preparation and application thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102417263A (en) * 2010-09-28 2012-04-18 中国石油化工股份有限公司 Method for processing wastewater from nitrochlorobenzene production
CN102417265A (en) * 2010-09-28 2012-04-18 中国石油化工股份有限公司 Method for effectively removing organic matters in wastewater from nitrochlorobenzene production
CN104923229A (en) * 2014-03-21 2015-09-23 中国科学院大连化学物理研究所 Activated carbon catalyst used for Fenton-like technology, and preparation and application thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108706772A (en) * 2018-06-08 2018-10-26 昆明理工大学 A kind of continuous treatment process of the waste water containing xanthate
CN115594357A (en) * 2022-11-08 2023-01-13 煤炭科学技术研究院有限公司（Cn） Acylation wastewater grading treatment method
CN115594357B (en) * 2022-11-08 2024-04-19 煤炭科学技术研究院有限公司 Fractional treatment method for acylated wastewater

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Application publication date: 20180424