CN108793552A - A kind of processing method of nigrosine production waste water - Google Patents
A kind of processing method of nigrosine production waste water Download PDFInfo
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- CN108793552A CN108793552A CN201810578008.4A CN201810578008A CN108793552A CN 108793552 A CN108793552 A CN 108793552A CN 201810578008 A CN201810578008 A CN 201810578008A CN 108793552 A CN108793552 A CN 108793552A
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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
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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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
- 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
- C02F1/048—Purification of waste water by evaporation
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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
- 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
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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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
- 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
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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
- 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
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F2001/007—Processes including a sedimentation step
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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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
- 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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
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Abstract
The invention discloses the processing methods that a kind of nigrosine produces waste water.This method comprises the following steps：(1) take nigrosine production waste water that condensation reaction occurs with formalin, reaction terminates filtering, obtains filtrate I；(2) pH value for the filtrate I that regulating step (1) obtains is 4~7, after Fenton's reaction, adjusts pH value to 9~11, further filters, obtain filtrate II；(3) heterogeneous catalyst is added in filtrate and carries out low-temperature atmosphere-pressure catalytic wet oxidation reaction；(4) treatment fluid that step (3) obtains further is subjected to MVR evaporation process desalinations.Formaldehyde condensation+Fenton's reaction+LCWO+ is steamed salt combination by the present invention, significantly reduces COD, aniline, ammonia nitrogen and the salt content in waste water, obvious processing effect.
Description
Technical field
The invention belongs to waste water technology fields, and the processing method of waste water is produced more particularly to a kind of nigrosine.
Background technology
Nigrosine, the molten Buddhist nun's lattice Rosin of alias oil-soluble nigrosine, alcohol soluble nigrosine, alcohol, is a kind of black dyes, for weaving
Dyeing on fibres.Since this dyestuff fastness to light and impermeability are upper similar to outstanding vat dye, have important
Value, is still used for textile dyeing and calico printing so far.
Nigrosine is to be aoxidized and obtained with aniline, and usual preparation method is to dissolve anilinechloride in the presence of mantoquita
So that it is aoxidized with sodium dichromate in the concentrated sulfuric acid and is made.Therefore, nigrosine production can discharge a large amount of toxic wastewaters, such waste water
In containing a large amount of chlorides, aniline category matter etc., there is higher COD and ammonia-nitrogen content.
Existing processing method be rectifying mode, by waste water moisture and part volatile organic matter be evaporated,
Aniline recovery；Then bottom liquid is through peroxide of iron flocculating setting；It is detached using filter press.However a series of above-mentioned processing procedures obtain
To water sample analysis result be still unable to reach the standard of direct emission.Water sample visually observes as dark brown, and in alkalinity, and salt contains
Amount, COD and ammonia-nitrogen content are still higher.
China application CN201410521666.1 discloses a kind of processing method of nigrosine production high-concentration salt-containing wastewater
And its processing system, including nigrosine production high-concentration salt-containing wastewater is passed through into alkali precipitation, extraction and filtering, to remove in waste water
Organic substance and suspension colloid；Pretreated nigrosine production high-concentration salt-containing wastewater is taken off by bipolar membrane device
Sodium chloride in waste water is converted into the hydrochloric acid and sodium hydroxide solution of respective concentration by salt treatment.This method is by removing
Salt is converted into certain density hydrochloric acid and sodium hydroxide solution, and reuse to front end alkali precipitation process has preferable desalination
Effect, but this method is not concerned with other noxious materials such as aniline category matter present in system.
To sum up, the present invention is directed to the defect of above-mentioned existing nigrosine wastewater treatment, develops a kind of nigrosine production waste water
Processing method, this method can effectively reduce COD value, ammonia-nitrogen content and the salt content of system, and processed waste water can reach
To discharge standard, be conducive to environmental protection.
Invention content
The purpose of the present invention is to provide the processing methods that a kind of nigrosine produces waste water.This method is by formaldehyde condensation+sweet smell
Reaction+LCWO the nigrosines that pause produce the processing method of waste water.
To achieve the above object, the present invention takes following technical scheme：
A kind of processing method of nigrosine production waste water, includes the following steps：
(1) take nigrosine production waste water that condensation reaction occurs with formalin, reaction terminates filtering, obtains filtrate I；
(2) pH value for the filtrate that regulating step (1) obtains is 4~7, after Fenton's reaction, adjusting pH value to 9~11, into
One step filters, and obtains filtrate II；
(3) heterogeneous catalyst is added in filtrate and carries out low-temperature atmosphere-pressure catalytic wet oxidation reaction；
(4) treatment fluid that step (3) obtains further is subjected to MVR evaporation process, obtains salt.
Preferably, for the nigrosine production waste water in the step (1) first successively through rectifying aniline recovery, iron oxide flocculation is heavy
Drop and filter press filtration step；
Preferably, it is 4~7 that hydrochloric acid is first added before carrying out condensation reaction and adjusts the pH of pretreated waste water for the step (1).
Preferably, in the step (1) formalin a concentration of 0.5~3%, condensation reaction be room temperature under carry out, instead
It is 1~4 hour between seasonable.
Preferably, first standing sedimentation is filtered again at room temperature after step (1) condensation reaction.
The aniline that standing sedimentation step can make unreacted complete and formaldehyde continue condensation, and to generate diaminodiphenylmethane yellowish
Color solid precipitates.
Preferably, the step (2) uses the pH value of alkaline solution regulation system, it is furthermore preferred that the alkaline solution is
The sodium hydroxide solution of 30~35wt% of mass fraction.
Preferably, the hydrogen peroxide and Fe that step (2) the Fenton's reaction reagent is 27.5% by mass fraction2+Composition, instead
It should be carried out at 30~60 DEG C, continuously stir 1~4h of reaction on the basis of the quality of filtrate I, H2O2Addition be 0.5%-
2%
Fenton oxidation：H2O2In Fe2+Catalytic action under produce hydroxyl radical free radical, with strong oxidizing property, Fenton examinations
Agent can aoxidize certain difficult to degrade and virose substance；Fenton reagent can generate molten iron complex compound when handling organic wastewater,
Flocculation can equally be played.
Low-temperature atmosphere-pressure catalytic wet oxidation (LCWO) can be urged using heterogeneous catalyst in a mild condition (low-temperature atmosphere-pressure)
Change H2O2It decomposes and generates the extremely strong OH free radicals of oxidability, the organic pollution in waste water is oxidized to less toxic or nontoxic
Small organic molecule is even direct oxidation into CO2And H2The inorganic matters such as O, leave no residue, and secondary pollution is small, and energy consumption is small, save operation
Expense.
Preferably, step (4) the low-temperature atmosphere-pressure catalytic wet oxidation is reacted under 30 DEG C~60 DEG C, normal pressure, instead
It is 1-4h between seasonable.
Preferably, step (5) the MVR evaporation process temperature is 80-110 DEG C.
After the present invention is handled, nigrosine produces the COD in waste water<1000mg/L, concentration of aniline<100mg/L, ammonia nitrogen
<100mg/L is practically free of salinity by evaporation process, and COD removal rates are up to 90% or more, and aniline removal rate is up to 99% or more, ammonia
85% or more nitrogen removal efficiency.
Present invention processing water outlet reaches country《Integrated wastewater discharge standard (GB8978-1996)》Discharge standard.
The present invention has following technical characterstic：
1) present invention steams salt joint technology using formaldehyde condensation+Fenton's reaction+LCWO+, can reduce COD in waste water,
Aniline, ammonia nitrogen and salt content, obvious processing effect.
2) polycondensation reaction of the present invention not only solves the secondary pollution being also easy to produce during nigrosine production wastewater treatment
Problem.
3) present invention uses two kinds of oxidation technologies of Fenton's reaction and LCWO simultaneously, can be by the organic pollution oxygen in waste water
Chemical conversion low toxicity or nontoxic small organic molecule are even direct oxidation into CO2And H2The inorganic matters such as O, leave no residue, secondary pollution
It is small, it is small compared to the processing method energy consumption that Fenton oxidation is used alone, save operating cost.
4) present invention can be recycled the salt in waste water, be economized on resources by MVR evaporation process.
Specific implementation mode
Following specific examples is the further explanation to method provided by the invention and technical solution, but is not construed as
Limitation of the present invention.
Embodiment 1：
One, the pretreatment of nigrosine production waste water
By nigrosine production waste water successively through rectifying aniline recovery, iron oxide flocculating setting and filter press filtration step,
Obtain pretreated waste water.
The water quality detection of pretreated waste water is as a result, referring to the following table 1.
Two, formaldehyde condensation is handled
It takes pretreated waste water that hydrochloric acid (37%) is added and adjusts pH=4~7, add 0.5~3% formalin, room temperature
Stirring, 1~4h of successive reaction are obtained by filtration filtrate, obtain filtrate I.
Three, Fenton's reaction
It is 4~7 or so that filtrate liquid caustic soda (30~35%NaOH), which adjusts pH value of solution, obtained by formaldehyde condensation, add 0.5~
2% hydrogen peroxide solution (27.5%) and 0.1~0.5% catalyst, and in 40~60 DEG C of waters bath with thermostatic control, react 1~4h, reaction
After pH value of solution 1~3 or so.Liquid caustic soda (30%NaOH) is added and adjusts pH to 9~11 or so, filtrate II is obtained by filtration.
Four, LCWO processing
Heterogeneous catalyst is added in filtrate after treatment and carries out low-temperature atmosphere-pressure catalytic wet oxidation reaction.
LCWO processing systems parameter is referring to table 2.
2 LCWO system fundamental reaction parameter lists of table
Five, salt steams
Processing water outlet carries out steaming salt experiment, stops experiment after measuring salt greatly.It is 104 DEG C to distill boiling temperature, measures salt greatly
116 DEG C of temperature, concentrate concentrate 25 times, it is pale to go out salt.
It see the table below by the parameters of above-mentioned steps treated condensed water：
| Detection project | Processed waste water |
| Appearance | Clear |
| Color | It is colourless |
| Density (g/mL) | 1.0 |
| PH value/acidity/basicity | 5~7 |
| Solid content (%) | 0 |
| COD(mg/L) | 60.2 |
| Ammonia nitrogen (mg/L) | 36.4 |
| Aniline | 0.5 |
Comparative example 1：
LCWO processing steps are omitted on the basis of embodiment 1, every by above-mentioned steps treated condensed water joins
Number is as follows：
The explanation of above example is only intended to help to understand the method for the present invention and its core concept.It should be pointed out that for
For those skilled in the art, without departing from the principle of the present invention, if can also be carried out to the present invention
Dry improvement and modification, these improvement and modification are also fallen into the claims in the present invention protection domain.
Claims (10)
1. a kind of processing method of nigrosine production waste water, which is characterized in that include the following steps：
(1) take nigrosine production waste water that condensation reaction occurs with formalin, reaction terminates filtering, obtains filtrate I；
(2) pH value for the filtrate I that regulating step (1) obtains is 4~7, after Fenton's reaction, adjusts pH value to 9~11, further
Filtering, obtains filtrate II；
(3) heterogeneous catalyst is added in filtrate II and carries out low-temperature atmosphere-pressure catalytic wet oxidation reaction；
(4) treatment fluid that step (3) obtains further is subjected to MVR evaporation process desalinations.
2. a kind of processing method of nigrosine production waste water as described in claim 1, which is characterized in that in the step (1)
Nigrosine production waste water first successively through rectifying aniline recovery, iron oxide flocculating setting and filter press filtration step.
3. a kind of processing method of nigrosine production waste water as described in claim 1, which is characterized in that the step (1) exists
It is 4~7 that hydrochloric acid is first added before progress condensation reaction and adjusts the pH of pretreated waste water.
4. a kind of processing method of nigrosine production waste water as described in claim 1, which is characterized in that in the step (1)
A concentration of the 0.5~3% of formalin, condensation reaction are to be carried out under room temperature, and the reaction time is 1~4 hour.
5. a kind of processing method of nigrosine production waste water as described in claim 1, which is characterized in that step (1) contracting
First standing sedimentation at room temperature after reaction is closed to be filtered again.
6. a kind of processing method of nigrosine production waste water as described in claim 1, which is characterized in that the step (2) is adopted
With the pH value of alkaline solution regulation system.
7. a kind of processing method of nigrosine production waste water as claimed in claim 6, which is characterized in that the alkaline solution is
The sodium hydroxide solution of 30~35wt%.
8. a kind of processing method of nigrosine production waste water as described in claim 1, which is characterized in that the step (2) is fragrant
The hydrogen peroxide and Fe that the reaction reagent that pauses is 27.5% by mass fraction2+Composition, reaction are carried out at 30 DEG C~60 DEG C, are continuously stirred
React 1h~4h；On the basis of the quality of filtrate I, H2O2Addition be 0.5%-2%.
9. a kind of processing method of nigrosine production waste water as described in claim 1, which is characterized in that the step (3) is low
Normal temperature and pressure catalytic wet oxidation is reacted under 30 DEG C~60 DEG C, normal pressure, reaction time 1-4h.
10. a kind of processing method of nigrosine production waste water as described in claim 1, which is characterized in that the step (4)
MVR evaporation process temperature is 80-110 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113104946A (en) * | 2021-04-01 | 2021-07-13 | 时代沃顿科技有限公司 | Method for treating wastewater containing polyamino aromatic compounds |
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| CN105923869A (en) * | 2016-05-03 | 2016-09-07 | 安徽南风环境工程技术有限公司 | Pretreatment method for chemical industry wastewater |
| CN106167332A (en) * | 2016-07-11 | 2016-11-30 | 浙江迪邦化工有限公司 | A kind of aniline intermediate produces the recycling processing method of waste water |
| CN106477769A (en) * | 2016-10-26 | 2017-03-08 | 浙江奇彩环境科技股份有限公司 | A kind of processing method of nitrobenzene compounds waste water |
| CN106882891A (en) * | 2017-03-30 | 2017-06-23 | 大丰跃龙化学有限公司 | A kind of method of wastewater treatment in cyclopropanecarboxylic acid production process |
-
2018
- 2018-06-07 CN CN201810578008.4A patent/CN108793552A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445711A (en) * | 2014-10-29 | 2015-03-25 | 绍兴奇彩化工有限公司 | Treatment method for aniline wastewater |
| CN104692576A (en) * | 2015-01-22 | 2015-06-10 | 绍兴奇彩化工有限公司 | Method for treating isatin wastewater |
| CN105923869A (en) * | 2016-05-03 | 2016-09-07 | 安徽南风环境工程技术有限公司 | Pretreatment method for chemical industry wastewater |
| CN106167332A (en) * | 2016-07-11 | 2016-11-30 | 浙江迪邦化工有限公司 | A kind of aniline intermediate produces the recycling processing method of waste water |
| CN106477769A (en) * | 2016-10-26 | 2017-03-08 | 浙江奇彩环境科技股份有限公司 | A kind of processing method of nitrobenzene compounds waste water |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113104946A (en) * | 2021-04-01 | 2021-07-13 | 时代沃顿科技有限公司 | Method for treating wastewater containing polyamino aromatic compounds |
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