CN105565416A - Treatment method of chlorobenzene apparatus wastewater - Google Patents
Treatment method of chlorobenzene apparatus wastewater Download PDFInfo
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- CN105565416A CN105565416A CN201410533330.7A CN201410533330A CN105565416A CN 105565416 A CN105565416 A CN 105565416A CN 201410533330 A CN201410533330 A CN 201410533330A CN 105565416 A CN105565416 A CN 105565416A
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Abstract
The invention provides a treatment method of chlorobenzene apparatus wastewater, and concretely relates to a method for carrying out adsorbing treatment on apparatus pretreatment wastewater by adopting metal supported active carbon. The method is characterized in that active carbon is modified, the modified active carbon is used in adsorbing treatment of the wastewater, desorption is carried out through blowing the above adsorbent with low pressure steam and nitrogen, benzene and chlorobenzene are recovered, and the desorbed adsorbent can be repeatedly used. The respective content of benzene and chlorobenzene in treated chlorobenzene wastewater is lower than 100ppm, the removal rate of organic matters reaches 90% or above, resources are saved, and the biochemical treatment cost of the wastewater is reduced.
Description
Technical field
The invention belongs to environmental technology field, be specifically related to the treatment process of Benzene Chloride trade effluent.
Background technology
Benzene Chloride is a kind of important basic organic synthesis raw material, as dyestuff, medicine, agricultural chemicals, organic synthesis intermediate.Industrial production mainly adopts benzene liquid phase chlorination method, domesticly generally adopts tower boiling continuous chlorination technique.The waste water produced in benzene chloride production process mainly comprises acid waste water, alkaline waste water and other waste water, and this composite waste has Cl
-the characteristics such as ionic concn is high, acidity is strong, colourity is dark, toxicity is large.If directly enter wastewater treatment field process, there is serious toxic action to the microorganism in sewage farm, greatly affect contaminant degradation rate.Common chlorobenzene waste water treatment process comprises the methods such as stripping, absorption, chemical treatment, biological treatment, although the waste water after stripping process can meet biochemical treatment requirement, but wherein also containing many benzene and Benzene Chloride, while adding cost for wastewater treatment, waste resource.
CN101186361A, CN101037245A adopt a kind of 3 D electrode reactor to carry out Benzene Chloride wastewater treatment, its method is that chlorobenzene waste water is introduced 3 D electrode reactor, setting electric current 1-5A, the residence time of waste water in 3 D electrode reactor is 30-120min, is directly discharged by tail water or do biochemical concentration process further after terminating.This technique is simple, but equipment requirements is high, and processing costs is high, and only relates to the process of lower concentration chlorobenzene waste water.
CN101391850A relates to the treatment process of Benzene Chloride and chloronitrobenzene producing wastewater microorganism, mainly utilize H.S.B. patent microbial strains, in conjunction with double oxygen system+aerobic system+BAC system process, even if successfully solve microorganism at total salt up under 25000mg/L, the rejection condition of chlorine ion concentration up to the multiple Toxic existence such as 30000mg/L and Benzene Chloride, nitro-chlorobenzene and oil of mirbane, process water still can reach the technical barrier of national grade one discharge standard, and produces without any residue biological sludge.This technological equipment investment is large, and complex process, technological difficulties are in the cultivation with microbial strains, and industrialization difficulty is large.
CN1559932A relates to chlorobenzene and the benzene method of wastewater treatment of overbasic, high chloride ion content, in distributing trough, intermediate pool buffering will be entered after preliminary sedimentation containing chlorobenzene and benzene waste water, squeeze in electrocatalysis device with pump, control the voltage and current of this device, after short stay, its water outlet cushions through intermediate pool, squeezing into after millipore filter filters through pump enters in equalizing tank again, discharges with after 98% sulfuric acid adjust ph.
The improvement of washing waste water and its recovery method as resource in CN1347849A benzene chloride production process, by waste water logical people's hydrogenchloride after filtering, steam benzene and Benzene Chloride simultaneously, and be separated, reclaim, improve acidity and waste water after removing benzene and Benzene Chloride passes through strongly basic anion exchange resin, to remove de-iron, effluent liquid is hydrochloric acid, the iron complex anion distilled water exchanged on strongly basic anion exchange resin elutes as regenerator, zeolite regeneration liquid is the liquor ferri trichloridi of high density, can make water purification agent, resin is then reproduced.This technological equipment investment is large, and complex technical process, difficult point is in the regeneration of exchange resin, and industrialization difficulty is large.
CN103754958A relates to a kind of technique utilizing the waste water of benzene chloride production to prepare iron oxide black, is specially: by the Fe in the washing waste acid water that produces in benzene chloride production
3+fe is reduced to reductive agent in reactor
2+, then add buck, make Fe
2+iron mud (Fe (OH is generated with alkali reaction
2)), then obtain iron mud solid through settling vat sedimentation, after compressor press filtration, be oxidized to iron oxide black (Fe in the basic conditions
3o
4); Clear water after the clear water on reactor top and the sedimentation of settling vat top is sent into resin column and is carried out Adsorption of Organic, then enters clear water treating pond and processes.This technique mainly make use of the iron ion in waste water, and organic process adopts resin absorption, but does not illustrate.
CN1023512979A relates to a kind of method of halogenated organic pollutant waste water process, joins containing in halogenated organic pollutant waste water, fully stirs 100-180h, effectively can process pollutent after sponge iron ball mill grinding is become particle; Or sponge iron and carrier be mixed and made into filler and add packing tower and carry out for organic pollutant wastewater process, residence time 20-40h, and requiring that halo organic pollutant is at 5-20mg/L, process range is limited.
CN101091922A relates to Nafion bag by the method for nano cuprous oxide and catalytic elimination Chlorobenzens thereof, chlorobenzene waste water is placed in lucifuge reactor, is equipped with glass and tetrafluoroethylene friction gear in reactor; Nafion bag is added by nano cuprous oxide with the ratio of 0.5g/L ~ 2.5g/L; Adopt additionaling power to make friction gear and Nafion wrap oxidized cuprous and glass and carry out mechanical friction.Adopt the method process Chlorobenzens, concentration is that the Chlorobenzens clearance in 10-100mg/L waste water can reach more than 80%.But operational condition is harsher, be difficult to realize industrialization.
In above technological method, there are some more serious technical problem or defects, such as operate loaded down with trivial details, processing cost is high, especially there is the high shortcoming of energy consumption in electrolytic process; Exploitation high efficiency, low cost process Benzene Chloride waster water process, to water conservation environment, promotes that the benign development of Benzene Chloride industry has strategic importance.
Summary of the invention
After the wastewater treatment of current Benzene Chloride device, still containing part benzene, Benzene Chloride and be unfavorable for the problem of biochemical treatment in waste water, the invention provides a kind for the treatment of process of Benzene Chloride waste water, to overcome the deficiencies in the prior art, in processed waste water, organic content obviously reduces, compare with existing treatment process, processing cost is lower, and operation is simpler.
Concrete treatment process key of the present invention is to use modified activated carbon absorbent, absorption pre-treatment post chlorization benzene waste water, after absorption, wastewater through organic matter clearance reaches more than 90%, reduce biochemical treatment cost, treating processes is simple, in recoverable wastewater, the organism such as benzene and Benzene Chloride, does not increase energy consumption in treating processes, does not produce new pollution.
Main technical schemes of the present invention:
Concrete treatment process key of the present invention is to have prepared high absorption property modified activated carbon absorbent, adopt adsorbent process Benzene Chloride waste water, effectively can reduce the content of benzene and Benzene Chloride in waste water, reach biochemical treatment requirement, reduce wastewater biochemical processing cost, then purge sorbent material respectively by low-pressure steam, nitrogen and can complete desorption.
It is characterized in that using metal load modified activated carbon to be sorbent material, waste water after the pre-treatment of adsorbing chlorinated benzene device; Purge sorbent material respectively with low-pressure steam, nitrogen again and carry out desorption, reclaim benzene and Benzene Chloride.Processed waste water organic removal rate reaches more than 90%, and water quality is limpid, recyclablely after sorbent material desorption applies mechanically.
The sorbent material adopted is modified activated carbon, and modified activated carbon is the granulated active carbon of supported copper or nickel, and loaded metal content is the 1%-5% of total mass, and granular size is 20-40 order.
The preparation method of described sorbent material is: granulated active carbon is placed in 0.1-0.5mol/L cupric ion or nickel ion solution; under normal temperature, flood 2-4h, after washing, filtering drying, and under nitrogen protection condition; in 300-500 DEG C of roasting temperature 2-3h, obtained sorbent material.
Described adsorbent amount is the 5%-10% of wastewater quality.
Benzene 0-1000ppm, chloride containing benzene 0-300ppm is contained in waste water after described pre-treatment.
Described adsorbent hydroxyl aluminum is 2-4h, adsorption temp 0-80 DEG C.
Described desorption temperature is 100-200 DEG C, holds time as 30-60min.
In Benzene Chloride waste water after the inventive method process, benzene and chlorobenzene content are all lower than 100ppm, and organic removal rate reaches more than 90%, have saved resource, reduce wastewater biochemical processing cost.
Embodiment
Below in conjunction with embodiment, the inventive method is described in detail.
Embodiment 1
Size 20 object 20g granulated active carbon is placed in 1L0.4mol/L copper nitrate solution, under normal temperature condition, stirs load 2h, after filter, washing, to dry, in 300 DEG C of roasting 2h under nitrogen protection condition, obtained modified gac (sorbent material).20g sorbent material is put in filler in packed column layer, under normal temperature condition, by 200g device pre-treatment post chlorization benzene waste water, (benzene content is 800mg/L, Benzene Chloride content is 300mg/L) pass through sorbent material with 1ml/min flow, processed waste water sampling analysis, benzene content is 43mg/L, Benzene Chloride content is 66mg/L, and organic removal rate is 90.1%.Respectively low-pressure steam, nitrogen are passed through sorbent material under 120 DEG C of conditions, control flow is 5ml/min, desorption is completed after maintaining 30min, adopt that same waste water, flow are constant carries out adsorption test again, processed waste water sampling analysis, benzene content is 38mg/L, and Benzene Chloride content is 67mg/L, and organic removal rate is 90.5%.After desorption, sorbent material still can be recycled again.
Embodiment 2
Size 30 object 20g granulated active carbon is placed in 1L0.3mol/L nickel nitrate solution, under normal temperature condition, stirs load 2h, after filter, washing, to dry, in 400 DEG C of roasting 2h under nitrogen protection condition, obtained modified gac (sorbent material).20g sorbent material is put in filler in packed column layer, under 40 DEG C of conditions, by 300g device pre-treatment post chlorization benzene waste water, (benzene content is 700mg/L, Benzene Chloride content is 200mg/L) pass through sorbent material with 2ml/min flow, processed waste water sampling analysis, benzene content is 35mg/L, Benzene Chloride content is 51mg/L, and organic removal rate is 90.4%.Respectively low-pressure steam, nitrogen are passed through sorbent material under 150 DEG C of conditions, control flow is 5ml/min, desorption is completed after maintaining 40min, adopt that same waste water, flow are constant carries out adsorption test again, processed waste water sampling analysis, benzene content is 40mg/L, and Benzene Chloride content is 48mg/L, and organic removal rate is 90.2%.After desorption, sorbent material still can be recycled again.
Embodiment 3
Size 40 object 40g granulated active carbon is placed in 1L0.5mol/L copper nitrate solution, under normal temperature condition, stirs load 4h, after filter, washing, to dry, in 500 DEG C of roasting 2h under nitrogen protection condition, obtained modified gac (sorbent material).40g sorbent material is put in filler in packed column layer, under 60 DEG C of conditions, by 600g device pre-treatment post chlorization benzene waste water, (benzene content is 1000mg/L, Benzene Chloride content is 260mg/L) pass through sorbent material with 3ml/min flow, processed waste water sampling analysis, benzene content is 44mg/L, Benzene Chloride content is 74mg/L, and organic removal rate is 90.6%.Respectively low-pressure steam, nitrogen are passed through sorbent material under 180 DEG C of conditions, control flow is 5ml/min, desorption is completed after maintaining 60min, adopt that same waste water, flow are constant carries out adsorption test again, processed waste water sampling analysis, benzene content is 49mg/L, and Benzene Chloride content is 73mg/L, and organic removal rate is 90.3%.After desorption, sorbent material still can be recycled again.
Claims (7)
1. a treatment process for Benzene Chloride device waste water, is characterized in that using metal load modified activated carbon to be sorbent material, waste water after the pre-treatment of adsorption treatment Benzene Chloride device; Purge sorbent material respectively with low-pressure steam, nitrogen again and carry out desorption, reclaim benzene and Benzene Chloride.
2. treatment process according to claim 1, it is characterized in that adopted sorbent material is modified activated carbon, modified activated carbon is the granulated active carbon of supported copper or nickel, and loaded metal content is the 1%-5% of total mass, and granular size is 20-40 order.
3. treatment process according to claim 1; it is characterized in that the preparation method of sorbent material is: granulated active carbon is placed in 0.1-0.5mol/L cupric ion or nickel ion solution; 2-4h is flooded under normal temperature; after washing, filtering drying; and under nitrogen protection condition; in 300-500 DEG C of roasting temperature 2-3h, obtained sorbent material.
4. treatment process according to claim 1, is characterized in that described adsorbent amount is the 5%-10% of wastewater quality.
5. treatment process according to claim 1, contains benzene 0-1000ppm, chloride containing benzene 0-300ppm in waste water after it is characterized in that pre-treatment.
6. treatment process according to claim 1, is characterized in that adsorbent hydroxyl aluminum is 2-4h, adsorption temp 0-80 DEG C.
7. treatment process according to claim 1, is characterized in that desorption temperature is 100-200 DEG C, holds time as 30-60min.
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| CN201410533330.7A CN105565416A (en) | 2014-10-11 | 2014-10-11 | Treatment method of chlorobenzene apparatus wastewater |
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| CN201410533330.7A CN105565416A (en) | 2014-10-11 | 2014-10-11 | Treatment method of chlorobenzene apparatus wastewater |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107855102A (en) * | 2016-09-22 | 2018-03-30 | 中国石油化工股份有限公司 | The preparation method and tail gas recycle purification method of Benzene Chloride tail gas adsorption agent |
| CN109999768A (en) * | 2019-05-05 | 2019-07-12 | 河北工业大学 | A kind of stalk base composite absorbent purified for chlorinated aromatic hydrocarbons in incineration flue gas |
Citations (2)
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| CN101260020A (en) * | 2008-04-15 | 2008-09-10 | 中国科学院山西煤炭化学研究所 | Method for treating benzene-containing waste water and reclaiming benzene |
| CN101314561A (en) * | 2007-06-02 | 2008-12-03 | 珠海醋酸纤维有限公司 | Adsorbent bed resolution method and adsorber for recycling acetone |
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2014
- 2014-10-11 CN CN201410533330.7A patent/CN105565416A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101314561A (en) * | 2007-06-02 | 2008-12-03 | 珠海醋酸纤维有限公司 | Adsorbent bed resolution method and adsorber for recycling acetone |
| CN101260020A (en) * | 2008-04-15 | 2008-09-10 | 中国科学院山西煤炭化学研究所 | Method for treating benzene-containing waste water and reclaiming benzene |
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| 刘芳: "活性炭吸附法处理苯系物及MTBE微污染废水的实验研究", 《中国优秀硕士学位论文全文数据库工程科技辑（月刊）》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107855102A (en) * | 2016-09-22 | 2018-03-30 | 中国石油化工股份有限公司 | The preparation method and tail gas recycle purification method of Benzene Chloride tail gas adsorption agent |
| CN109999768A (en) * | 2019-05-05 | 2019-07-12 | 河北工业大学 | A kind of stalk base composite absorbent purified for chlorinated aromatic hydrocarbons in incineration flue gas |
| CN109999768B (en) * | 2019-05-05 | 2020-01-07 | 河北工业大学 | Straw-based composite adsorbent for purifying chlorinated aromatic hydrocarbons in incineration flue gas |
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