CN106186147A - A kind of recovery and treatment method of high concentration waste organic acid - Google Patents
A kind of recovery and treatment method of high concentration waste organic acid Download PDFInfo
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- CN106186147A CN106186147A CN201610595824.7A CN201610595824A CN106186147A CN 106186147 A CN106186147 A CN 106186147A CN 201610595824 A CN201610595824 A CN 201610595824A CN 106186147 A CN106186147 A CN 106186147A
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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
- C02F1/26—Treatment of water, waste water, or sewage by extraction
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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
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- C02F2101/34—Organic compounds containing oxygen
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Abstract
Invention provides the recovery and treatment method of a kind of high concentration waste organic acid.Described recovery and treatment method is with complexing extractant, described high concentration waste organic acid to be carried out complexometric extraction under sour environment, obtains extraction phase and aqueous phase after stratification；Subsequently, to the described extraction phase addition parsing agent obtained to carry out complexing extractant regeneration, stratification after hybrid reaction, it is thus achieved that the concentrated solution containing organic acid and regeneration complexing extractant.Recovery and treatment method of the present invention can reclaim the organic acid raw material in waste water simultaneously, and directly set is used for production process.And the waste water after recovered process can directly carry out routine biochemistry process, stably reaching standard discharges.
Description
Technical field
The present invention relates to Fine Chemistry Wastewater process field, particularly to the recycling of a kind of high concentration waste organic acid
Method.
Background technology
Organic acid refers to that some have the organic compound of acidity.The machine acid of common are is carboxylic acid, and its acidity comes from carboxyl
(-COOH).Kinds of organic acids is various, and is widely used.Some of which organic acid be used as synthesis medicine and pesticide raw material and
Intermediate.Therefore, along with medicine and the production of pesticide, can produce the multiple waste water containing high concentration organic acid, this waste water is organic
Substrate concentration is high, and mostly has bio-toxicity, causes biochemical system disorderly, the even mortality of activated sludge.
The most conventional method processing organic acid wastewater has physico-chemical process, chemical oxidization method, membrane separation technique and biochemical process.
Patent CN102942281 B discloses the processing method of a kind of high concentration mixed organic acid waste water, and invention is for maleic anhydride production system
The high concentration mixed organic acid waste water that system produces, uses two grades of flocculation sediments-secondary membrane separation-evaporation and concentration process integration route
Processing, the waste water after process reaches national grade one discharge standard.In invention, two grades of flocculations separate alternately with secondary membrane, flocculation
Process adds flocculant kind up to 7 kinds, and uses the multiple filtration sides such as sand filtration, property charcoal filtration, ultrafiltration, nanofiltration, reverse osmosis that live
Formula, not only processes technique very complicated, and invest, run, cost of equipment maintenance high, do not possess industrial prospect.
Patent CN101570381A discloses a kind of organic acid wastewater treatment method and system, and invention is for PTA acetic acid
Waste water, uses anaerobic-aerobic to process successively in acid condition.Decrease the neutralization alkali number of waste water.The method application model
It is with limit, acetic acid is more adapted to, it is difficult to effectively process chemical constitution complexity and there is the organic acid wastewater of bio-toxicity.
It would therefore be desirable to a kind of new processing method, it is possible to effectively reclaim organic acid from waste water, reach waste water without
Poison, the effect of recycling.
Summary of the invention
It is an object of the invention to provide the recovery and treatment method of a kind of high concentration waste organic acid, can reclaim useless simultaneously
Organic acid raw material in water, and directly set is used for production process.And the waste water after recovered process can directly carry out routine biochemistry
Processing, stably reaching standard discharges.
To achieve these goals, present invention firstly provides the recovery and treatment method of a kind of high concentration waste organic acid, institute
The method of stating is with complexing extractant, described high concentration waste organic acid to be carried out complexometric extraction, after stratification under sour environment
Obtain extraction phase and aqueous phase；Subsequently, to the described extraction phase addition parsing agent obtained to carry out complexing extractant regeneration, mixing is anti-
Should stratification afterwards, it is thus achieved that the concentrated solution containing organic acid and regeneration complexing extractant；Wherein, described complexing extractant includes complexation
Agent and diluent, one or both in trioctyl phosphine oxide or N-Laurel (trialkyl methyl) amine of described chelating agent mix
Close, described diluent one in aerial kerosene or diesel oil.
In an embodiment of the present invention, described chelating agent accounts for the 24～48% of described complexing extractant volume.
In an embodiment of the present invention, described parsing agent is sodium hydroxide solution.Preferably, described sodium hydroxide solution
Mass fraction is 12%.
In an embodiment of the present invention, described complexing extractant gives up with described high concentration waste organic acid high concentration organic acid
The volume ratio of water is 1:(5～8).
In an embodiment of the present invention, in described complexing extractant regenerates, described sodium hydroxide solution and described extraction
The volume ratio of phase is 1:(4～6).
In an embodiment of the present invention, described sour environment refers to that pH value is in the range of 3～5.
In an embodiment of the present invention, described complexing extractant reacts with the complexometric extraction of described high concentration waste organic acid
Time is 30～60 minutes.
In an embodiment of the present invention, during the complexing extractant regenerative response of described extraction phase and described sodium hydroxide solution
Between be 30～60 minutes.
In a preferred embodiment of the present invention, it is provided that the recovery and treatment method of a kind of high concentration waste organic acid, described side
Method comprises the following steps: S10. complexometric extraction: regulate the pH value of described high concentration waste organic acid, makes described high concentration organic acid
The pH value of waste water is between 3～5, using chelating agent and diluent mixed liquor as complexing extractant, with described complexing extractant with
The volume ratio of described high concentration waste organic acid is 1:(5～8) ratio add described in described high concentration waste organic acid
Complexing extractant, complexometric extraction reacts 30～60 minutes, and stratification obtains extraction phase and aqueous phase；Step S20. complexing extractant
Regeneration: take the described extraction phase that step S10 obtains, with resolve agent and described extraction phase volume ratio as 1:(4～6) ratio
Example, adds described parsing agent, hybrid reaction 30～stratification after 60 minutes to described extraction phase, and lower floor is containing organic acid
Concentrated solution, upper strata is regeneration complexing extractant；Wherein, described parsing agent be mass fraction be the sodium hydroxide solution of 12%.
In an embodiment of the present invention, described chelating agent accounts for the 24～48% of described complexing extractant volume.
In an embodiment of the present invention, the described concentrated solution part containing organic acid can be back to chemical process, institute
State regeneration complexing extractant and then can be re-used for step S10.
In the present invention by choosing suitable extractant and complexometric extraction technique so that through processing method of the present invention
The COD clearance of the high concentration waste organic acid after process is 50～70%, and organic acid clearance is up to 99%.Through institute of the present invention
State the described high concentration waste organic acid (i.e. described aqueous phase in step S10) after method processes and there is biodegradability, raw through A/O
After change processes, indices can reach " integrated wastewater discharge standard " (GB8978-96) one-level.Furthermore, in the method for the invention
In described complexing extractant can also recycle, both stopped the secondary pollution problem that produces because waste water processes, entered again
One step reduces the cost that waste water processes.
Compared with prior art, the described recovery and treatment method of the present invention has the advantage that
1, the clearance of organic acid is up to 99%, and COD clearance, up to 50～70%, improves the biodegradability of waste water,
Guarantee that subsequent biochemical treatment effect is stable, bio-chemical effluent qualified discharge.
2, from waste water extract the concentrated solution containing organic acid, be mainly composed of pivalic acid, (R)-(+)-2-(4-oxybenzene
Epoxide) the difficult degradation organic acid such as propanoic acid, time acid, can be as producing the raw material of pesticide intermediate, and direct reuse is in production
Workshop section, thus reduce production cost, there is obvious economic benefit.
3, operational approach of the present invention simple, without heating up, equipment investment and operating cost are low, meet wanting of energy-conserving and environment-protective
Ask, there is preferable industrialized popularization value.
Detailed description of the invention
Hereinafter, in conjunction with detailed description of the invention, the technology of the present invention is described in detail.It is appreciated that the various following tool
Body embodiment is only used for helping skilled in the art to understand the present invention, rather than limitation of the present invention.
Embodiment 1
In the present embodiment, it is provided that the recovery and treatment method of a kind of high concentration waste organic acid, the spy of Zhejiang pharmaceutical factory
Valeric chloride workshop, hereinafter referred to as pivaloyl chloride waste water, raw water quality situation: pH=3, COD:41035mg/L, pivalic acid is dense
Degree: 13855mg/L, has penetrating odor.
Described method specifically includes following steps.
Step S10. complexometric extraction: first, in the present embodiment, with trioctyl phosphine oxide as extractant, with aerial kerosene
For diluent, described trioctyl phosphine oxide is 1:4 with the volume ratio of described aerial kerosene, obtains complexation extraction after both mix homogeneously
Take agent.Taking pivaloyl chloride waste water described in 3L, add the above-mentioned complexing extractant of 600mL, hybrid reaction is stratification after 30 minutes, obtains
Obtain extraction phase and aqueous phase.Described extraction phase is sent into extractant regeneration device and is regenerated, after described aqueous phase is removing pivalic acid
Waste water, sample analysis.
The regeneration of step S20. complexing extractant: the described extraction phase that step S10 is obtained and the hydrogen of mass fraction 12%
Sodium hydroxide solution 5:1 by volume adds in described extractant regeneration device, reacts 30 minutes, standing, split-phase, it is thus achieved that regeneration extraction
Take agent and organic acid dope.The composition main pivalic acid sodium of described organic acid dope, concentration is 351066mg/L, is equivalent to quality
Mark about 35%, can be back to pivaloyl chloride as raw materials for production and produce workshop section.Extractant after regeneration is back to step S10
In.
Detection processed waste water (aqueous phase i.e. obtained in step S10) water quality: COD:12085mg/L, clearance is
70.5%；Pivalic acid concentration: 40mg/L, clearance 99.7%.This water quality has biodegradability, every after A/O biochemical treatment
Index can reach " integrated wastewater discharge standard " (GB8978-96) one-level.
Embodiment 2
In the present embodiment, it is provided that a kind of method removing aniline category matter from high concentration waste organic acid, it is right to process
As take from (R) of Shandong insecticide factory-(+)-2-(4-oxybenzene epoxide) methyl propionate workshop, hereinafter referred to as (R)-(+)-2-(4-
Oxybenzene epoxide) methyl propionate waste water, raw water quality situation: pH=7, COD:24490mg/L, (R)-(+)-2-(4-oxybenzene epoxide)
Propionate concentration: 6704mg/L.
Described method specifically includes following steps.
Step S10. complexometric extraction: first, in the present embodiment, with N-Laurel (trialkyl methyl) amine as extractant, with
Diesel oil is diluent, and described N-Laurel (trialkyl methyl) amine is 24:76 with the volume ratio of described diesel oil, after both mix homogeneously
Obtain complexing extractant.Take (R) described in 3L-(+)-2-(4-oxybenzene epoxide) methyl propionate waste water, regulate its pH value 3～5 it
Between, adding the above-mentioned complexing extractant of 500mL, hybrid reaction is stratification after 60 minutes, it is thus achieved that extraction phase and aqueous phase.Described extraction
Send into extractant regeneration device mutually to regenerate, described aqueous phase be removing (R)-(+) giving up after-2-(4-oxybenzene epoxide) propanoic acid
Water, sample analysis.
The regeneration of step S20. complexing extractant: the described extraction phase that step S10 is obtained and the hydrogen of mass fraction 12%
Sodium hydroxide solution 5:1 by volume adds in described extractant regeneration device, reacts 30 minutes, standing, split-phase, it is thus achieved that regeneration extraction
Take agent and organic acid dope.The composition of described organic acid dope predominantly (R)-(+)-2-(4-oxybenzene epoxide) sodium propionate, concentration
For 195530mg/L, be equivalent to mass fraction about 25%, can be back to as raw materials for production (R)-(+)-2-(4-oxybenzene epoxide)
Methyl propionate produces workshop section.Extractant after regeneration is back to waste water extraction next time.
Detection processed waste water (aqueous phase i.e. obtained in step S10) water quality: COD:6483mg/L, clearance 73.5%；
(R)-(+)-2-(4-oxybenzene epoxide) propionate concentration: 10mg/L, clearance 99.8%.This water quality has biodegradability, raw through A/O
After change processes, indices can reach " integrated wastewater discharge standard " (GB8978-96) one-level.
Embodiment 3
In the present embodiment, it is provided that a kind of method removing aniline category matter from high concentration waste organic acid, it is right to process
As taking from the Biphenthrin workshop of Jiangsu insecticide factory, hereinafter referred to as Biphenthrin waste water, raw water quality situation: pH=3,
COD:49606mg/L, time acid concentration: 10399mg/L, have penetrating odor.
Described method specifically includes following steps.
Step S10. complexometric extraction: first, in the present embodiment, with trioctyl phosphine oxide as extractant, with aerial kerosene
For diluent, described trioctyl phosphine oxide and aerial kerosene volume ratio are 48:52, obtain complexometric extraction after both mix homogeneously
Agent.Taking Biphenthrin waste water described in 3L, add the above-mentioned complexing extractant of 600mL, hybrid reaction is stratification after 45 minutes, it is thus achieved that
Extraction phase and aqueous phase.Described extraction phase is sent into extractant regeneration device and is regenerated, after described aqueous phase is removing time acid
Waste water, sample analysis.
The regeneration of step S20. complexing extractant: the described extraction phase that step S10 is obtained and the hydrogen of mass fraction 12%
Sodium hydroxide solution 4:1 by volume adds in described extractant regeneration device, reacts 30 minutes, standing, split-phase, it is thus achieved that regeneration extraction
Take agent and organic acid dope.The composition of described organic acid dope is mainly apthol AS-LC, and concentration is time acid sodium, and concentration is
207980mg/L, is equivalent to mass fraction about 20%, can be back to Biphenthrin as raw materials for production and produce workshop section.After regeneration
Extractant is back to waste water extraction next time.
Detection processed waste water (aqueous phase i.e. obtained in step S10) water quality: COD:23655mg/L, clearance 52.3%；
Time acid concentration: 15mg/L, clearance 99.8%.This water quality has biodegradability, after A/O biochemical treatment indices up to
To " integrated wastewater discharge standard " (GB8978-96) one-level.
Embodiment 4
In the present embodiment, it is provided that a kind of method removing aniline category matter from high concentration waste organic acid, it is right to process
As same as in Example 1.
Described method specifically includes following steps.
Step S10. complexometric extraction: first, in the present embodiment, with N-Laurel (trialkyl methyl) amine as extractant, with
Aerial kerosene is diluent, and described DBBP and diesel fuel volume ratio for 3:7, obtains complexation extraction after both mix homogeneously
Take agent.Taking pivaloyl chloride waste water described in 3L, add the above-mentioned complexing extractant of 400mL, hybrid reaction is stratification after 30 minutes, obtains
Obtain extraction phase and aqueous phase.Described extraction phase is sent into extractant regeneration device and is regenerated, after described aqueous phase is removing pivalic acid
Waste water, sample analysis.
The regeneration of step S20. complexing extractant: the described extraction phase that step S10 is obtained and the hydrogen of mass fraction 12%
Sodium hydroxide solution 4:1 by volume adds in described extractant regeneration device, reacts 60 minutes, standing, split-phase, it is thus achieved that regeneration extraction
Take agent and organic acid dope.The composition of described organic acid dope is mainly pivalic acid sodium, and concentration is 329760mg/L, is equivalent to matter
Amount mark about 33%, can be back to pivaloyl chloride as raw materials for production and produce workshop section.It is useless that extractant after regeneration is back to next time
Water extracts.
Detection processed waste water (aqueous phase i.e. obtained in step S10) water quality: COD:12474mg/L, clearance 69.6%；
Pivalic acid concentration: 42mg/L, clearance 99.7%.This water quality has biodegradability, after A/O biochemical treatment indices up to
To " integrated wastewater discharge standard " (GB8978-96) one-level.
Embodiment 5
In the present embodiment, it is provided that a kind of method removing aniline category matter from high concentration waste organic acid, it is right to process
As for (R)-(+)-2-(4-oxybenzene epoxide) methyl propionate waste water, raw water quality: pH=7, COD:24490mg/L, (R)-(+)-
2-(4-oxybenzene epoxide) propionate concentration: 6704mg/L.
Described method specifically includes following steps.
Step S10. complexometric extraction: first, in the present embodiment, with trioctyl phosphine oxide as extractant, is dilute with diesel oil
Releasing agent, described trioctyl phosphine oxide and diesel fuel volume ratio for 28:72, obtains complexing extractant after both mix homogeneously.Take 3L institute
State (R)-(+)-2-(4-oxybenzene epoxide) methyl propionate waste water, regulate its pH value between 3～5, add 450mL above-mentioned complexation extraction
Taking agent, hybrid reaction is stratification after 45 minutes, it is thus achieved that extraction phase and aqueous phase.Described extraction phase is sent into extractant regeneration device and is entered
Row regeneration, described aqueous phase be removing (R)-(+) waste water after-2-(4-oxybenzene epoxide) propanoic acid, sample analysis.
The regeneration of step S20. complexing extractant: the described extraction phase that step S10 is obtained and the hydrogen of mass fraction 12%
Sodium hydroxide solution 6:1 by volume adds in described extractant regeneration device, reacts 30 minutes, standing, split-phase, it is thus achieved that regeneration extraction
Take agent and organic acid dope.The composition of described organic acid dope predominantly (R)-(+)-2-(4-oxybenzene epoxide) sodium propionate, concentration
For 195530mg/L, be equivalent to mass fraction about 20%, can be back to as raw materials for production (R)-(+)-2-(4-oxybenzene epoxide)
Methyl propionate produces workshop section.Extractant after regeneration is back to waste water extraction next time.
Detection processed waste water (aqueous phase i.e. obtained in step S10) water quality: COD:6591mg/L, clearance 73.1%；
(R)-(+)-2-(4-oxybenzene epoxide) propionate concentration: 15mg/L, clearance 99.8%.This water quality has biodegradability, raw through A/O
After change processes, indices can reach " integrated wastewater discharge standard " (GB8978-96) one-level.
In the present invention by choosing suitable extractant and complexometric extraction technique so that through processing method of the present invention
The COD clearance of the high concentration waste organic acid after process is 50～70%, and organic acid clearance is up to 99%.Through institute of the present invention
State the described high concentration waste organic acid (i.e. described aqueous phase in step S10) after method processes and there is biodegradability, raw through A/O
After change processes, indices can reach " integrated wastewater discharge standard " (GB8978-96) one-level.Furthermore, in the method for the invention
In described complexing extractant can also recycle, both stopped the secondary pollution problem that produces because waste water processes, entered again
One step reduces the cost that waste water processes.
The present invention is been described by by above-mentioned related embodiment, but above-described embodiment is only the example implementing the present invention.
It must be noted that, it has been disclosed that embodiment be not limiting as the scope of the present invention.On the contrary, be contained in the spirit of claims
And the amendment of scope and equalization arrange and are all included in the scope of the present invention.
Claims (9)
1. the recovery and treatment method of a high concentration waste organic acid, it is characterised in that described recovery and treatment method is in acidity
With complexing extractant, described high concentration waste organic acid is carried out complexometric extraction under environment, after stratification, obtain extraction phase and water
Phase；Subsequently, to the described extraction phase addition parsing agent obtained to carry out complexing extractant regeneration, stratification after hybrid reaction,
Obtain the concentrated solution containing organic acid and regeneration complexing extractant；Wherein, described complexing extractant includes chelating agent and diluent, institute
Stating chelating agent one or both mixing in trioctyl phosphine oxide or N-Laurel (trialkyl methyl) amine, described diluent selects
One in aerial kerosene or diesel oil.
2. the method for claim 1, it is characterised in that described chelating agent account for described complexing extractant volume 24～
48%.
3. the method for claim 1, it is characterised in that described parsing agent is sodium hydroxide solution.
4. the method for claim 1, it is characterised in that described complexing extractant is high with described high concentration waste organic acid
The volume ratio of concentration organic acid wastewater is 1:(5～8).
5. the method for claim 1, it is characterised in that in described complexing extractant regenerates, described parsing agent and institute
The volume ratio stating extraction phase is 1:(4～6).
6. the method for claim 1, it is characterised in that described sour environment refers to that pH value is in the range of 3～5.
7. method as claimed in claim 3, it is characterised in that the mass fraction of described sodium hydroxide solution is 12%.
8. the method for claim 1, it is characterised in that described complexing extractant and described high concentration waste organic acid
The complexometric extraction response time is 30～60 minutes.
9. the method for claim 1, it is characterised in that described extraction phase regenerates with the complexing extractant of described parsing agent
Response time is 30～60 minutes.
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