CN110282798A - A kind of processing method of synthesizing substituted and imidazoles organic wastewater - Google Patents
A kind of processing method of synthesizing substituted and imidazoles organic wastewater Download PDFInfo
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Abstract
The invention discloses a kind of processing methods of synthesizing substituted and imidazoles organic wastewater.The processing method includes the following steps: the alcohols material in S1. separation and recovery organic wastewater；S2. organic acid is separated and recovered, organic acid and recycling mother liquor are obtained；S3. aniline is separated and recovered；S4. the separation waste liquid Fenton process deep oxidation in S3 is flocculated, separates supernatant, sewage treatment plant is sent in water outlet after decolorization adsorption removal.Synthesizing substituted and imidazoles the organic wastewater that the present invention is handled is the organic wastewater of the alcohols containing high concentration, organic acid and aniline, and wherein the concentration of alcohols is 30~40%, and the concentration of organic acid is 2~3%, and the concentration of aniline is 1~2%.Processing method of the invention is using the hard-degraded substance in Fenton process deep oxidation waste water, then settles through activated carbon adsorption, and COD range is 90~400mg/L after processing, and coloration is 10~50.Processing method of the invention has effectively recycled alcohols, organic acid and aniline ingredient simultaneously, and the rate of recovery of alcohols is 100%, and the rate of recovery of organic acid is 95~98%, and the rate of recovery of aniline is 90%~95%.
Description
Technical field
The present invention relates to wastewater from chemical industry technical fields, more particularly, to a kind of synthesizing substituted and imidazoles organic waste
The processing method of water.
Background technique
With the lasting development of industry, various organic solvents and chemical synthesis organic matter are widely used, also therefore serious
Polluted natural environment, country is also more and more stringent to the emission request of wastewater from chemical industry to environmental issue pay attention to day by day.Therefore
How a great problem that these pollutants be now wastewater processing technology is effectively removed.
Contain organic solvent alcohols in synthesizing substituted and imidazoles organic wastewater, there are also the raw material aniline not reacted completely
And organic acid, and these three types of material concentrations are relatively high.It is Fenton that the prior art, which handles industrial organic waste water and applies at most,
Method, but Fenton process is when handling synthesizing substituted and imidazoles organic wastewater, there are Fenton reagent consumption is big, at high cost, nothing
Method recycles the useful raw material in waste water, and is difficult to the COD of waste water being down to discharge standard.Prior art CN108439671A is disclosed
A kind of photovoltaic drives electric Fenton from the system of maintenance and the method for aniline degradation waste water, secondly for the processing side containing aniline waste water
Method is Fenton facture, and theing improvement is that improves former Fenton system for handling, is driven to Fenton processing body using photovoltaic
System provides renewable energy, the whole effect for promoting Fenton processing.
Therefore, synthesizing substituted and imidazoles organic wastewater can be effectively treated it is contemplated that finding one kind in this field,
Related Fenton processing cost is reduced, the processing method of discharge of wastewater COD is reduced.
Summary of the invention
It is especially synthesizing substituted and imidazoles the technical problem to be solved by the present invention is to overcome existing aniline organic wastewater
Treatment of Organic Wastewater COD value is higher, the organic matter rate of recovery low defect and deficiency, and providing a kind of synthesizing substituted and imidazoles has
The processing method of machine waste water.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
The processing method of a kind of synthesizing substituted and imidazoles organic wastewater, includes the following steps:
S1. the alcohols material in organic wastewater is separated and recovered, pure and mild recycling mother liquor is obtained；
S2. the recycling mother liquor in S1 is further separated and recovered into organic acid, obtains organic acid and recycling mother liquor；
S3. the recycling mother liquor in S2 is further separated and recovered into aniline, obtains aniline and separation waste liquid；
S4. the separation waste liquid Fenton process deep oxidation in S3 being flocculated, separates supernatant, active carbon decolorization adsorption removes,
Sewage treatment plant is sent in water outlet.
Alcohols containing high concentration, organic acid and aniline in synthesizing substituted and imidazoles organic wastewater, wherein alcohols
Concentration is 30~40%, and the concentration of organic acid is 2~3%, and the concentration of aniline is 1~2%.
The present invention first recycles the alcohols material in waste water, then the organic acid in recycling waste water recycles the benzene in waste water
Amine, the organic matter in residual waste solution are flocculated using Fenton process deep oxidation, are most removed afterwards through decolorization adsorption, are reduced COD value and are reached
Downstream garden sewage treatment plant adapter tube standard, COD value can be reduced to 90~460mg/L.Four step rule of the invention handles synthesis
The organic wastewater of substituted benzimidazole has sufficiently recycled useful raw material and the solvent in waste water, had both saved compared with existing Fenton process
Saved the production cost of substituted benzimidazole, further, recycled the ingredients such as acid, alcohol and aniline early period, these ingredients without
Fenton reagent treatment, which need to be consumed, reduces the difficulty of later period Fenton process processing waste water, has high economic benefit, is suitble to industry
Wastewater treatment.
The present invention first recycles the alcohols material in waste water, then the organic acid in recycling waste water recycles the benzene in waste water
Amine, due to highest containing determining alcohol in waste water of the invention, and organic acid and aniline are soluble in alcohols, therefore first pass through distillation point
Alcohols is separated out, the presence because of alcohols is avoided to reduce the recovery efficiency of organic acid and aniline.Similarly, aniline itself is insoluble in water, just
It is due to, containing the raw material organic acid that unreacted is complete, just increasing the solubility and recovery difficult of aniline, therefore second in waste water
Step recycling organic acid, last aniline recovery.Therefore, the recycling sequence of alcohols material of the invention, organic acid and aniline is to final
Water treatment effect and the organic matter rate of recovery be also extremely important.
Wherein, the alcohols of processing method of the invention recycling includes: methanol, ethyl alcohol, isopropanol；
The organic acid of recycling includes: positive valeric acid, n-caproic acid, positive enanthic acid, caprylic acid；
The aniline of recycling includes: aniline, o-phenylenediamine, p-phenylenediamine, m-phenylene diamine (MPD).
Preferably, the separation and recovery method of alcohols material described in S1 are as follows: distill to obtain containing 50~60% by organic wastewater
The fraction of alcohols, fraction is again through the alcohols material in rectifying recycling waste water.It such as can be the fraction of 50% or 60% alcohols.
The separation and recovery of alcohols material of the invention is distillation-rectifying recycling, distill out be alcohols and water mixed fraction,
With the extension of distillation time, vapo(u)rizing temperature is higher, and the concentration of alcohol is lower and lower, when not alcohol-containing in the fraction steamed, has steamed
Alcohol-containing 50~60% in fraction solution out can pass through the content of alcohol in gas chromatographic detection fraction.
Preferably, the method for organic acid is separated and recovered described in S2 are as follows: the recycling mother liquor in S1 is adjusted into pH to 3~6, is added
Enter salting-out agents, separate upper layer organic acid, recycles the organic acid in waste water.Such as can by the recycling mother liquor in S2 adjust pH to 3,
4 or 5.
Preferably, the method for aniline is separated and recovered described in S3 are as follows: the recycling mother liquor in S2 is adjusted into pH value to 9~12,
Extractant is added to extract, aniline is precipitated in separating and extracting layer, vacuum distillation, recycles the aniline in waste water.Such as it can be by returning in S2
It receives mother liquor and adjusts pH value to 10,11 or 12.
The present invention recycles organic acid using saltouing, wherein salting-out agents can for sodium chloride, sodium sulphate, potassium chloride, potassium sulfate,
Ammonium chloride or ammonium sulfate, salting-out agents additional amount are 1~3g/L.Such as salting-out agents additional amount can be 1g/L, 2g/L or 3g/L, have
The rate of recovery of machine acid can achieve 95~98%.
The present invention uses extraction and recovery aniline, and extractant can be with are as follows: chloroform or methylene chloride.The recovery of extraction of aniline can
To reach 90~95%.
Preferably, the flocculated concrete operations of Fenton process deep oxidation described in S4 are as follows: adjust separation waste liquid pH value be 2~
5, FeSO is added4·7H2The H of O and mass fraction 30%2O2Hard-degraded substance in deep oxidation residual waste solution, adjusting pH value is
7~9, flocculant and flocculation aid, flocculation sedimentation is added.Such as the pH value of adjustable separation waste liquid is 3,4 or 5, pH after oxidation
Value can be 7 or 8.
Preferably, the FeSO4·7H2The additional amount of O is 3~5g/L, 30%H2O2Additional amount is 30~50mL/L.
It is highly preferred that the reaction temperature of the Fenton process deep oxidation is 35~50 DEG C, 1~2h of reaction time.
Preferably, the flocculant is the flocculant PAC aqueous solution that mass fraction is 1%~3%, and flocculation aid is quality point
The PAM aqueous solution that number is 0.1%~0.5%.
It is highly preferred that the additive amount of the flocculant PAC aqueous solution is 0.5~2g/L, the addition of flocculation aid PAM aqueous solution
Amount is 0.5~4g/L.Above-mentioned dosage is on the basis of the volume of waste liquid.
Preferably, decolorization adsorption is active carbon decolorization adsorption, and activated carbon particle size is 100~300 mesh, and active carbon additional amount is
1~5g/L.Better adsorption bleaching effect may be implemented in 100~300 mesh in activated carbon particle size control.
Compared with prior art, the beneficial effects of the present invention are:
(1) synthesizing substituted and imidazoles the organic wastewater that handles of the present invention be the alcohols containing high concentration, organic acid and
The organic wastewater of aniline, wherein the concentration of alcohols is 30~40%, and the concentration of organic acid is 2~3%, the concentration of aniline is 1~
2%.
(2) the processing method first step of the invention is by distilling, rectifying, the solvent alcohols material in recycling waste water, and second
Step realizes useful original in waste water by the aniline in extraction and recovery waste water by the organic acid recycled in waste water of saltouing, third step
The recycling and reusing of material had both saved synthesizing substituted and imidazoles production cost, and it is useless to also reduce the processing of later period Fenton process
The difficulty of water.
(3) processing method of the invention is using the hard-degraded substance in Fenton process deep oxidation waste water, then inhales through active carbon
The COD value and coloration of waste water is greatly reduced in attached sedimentation, and COD range is 90~460mg/L, and coloration is 10~50.
(4) processing method of the invention has effectively recycled alcohols, organic acid and aniline ingredient simultaneously, and the rate of recovery of alcohols is
100%, the rate of recovery of organic acid is 95~98%, and the rate of recovery of aniline is 90~95%.
Specific embodiment
The present invention is further illustrated With reference to embodiment, but embodiment the present invention is not done it is any
The restriction of form.Unless otherwise indicated, source chemicals used in the embodiment of the present invention are the source chemicals routinely bought.
Wherein synthesizing substituted and imidazoles the basic content of organic wastewater such as the following table 1 of the invention:
Table 1
| Classification | Alcohols/% | Organic acid/% | Aniline/% | COD mg/L | Coloration |
| Waste water stoste | 30~40 | 2~3 | 1~2 | 450000~500000 | 300~400 |
The wherein detection method of COD are as follows: HJ/T 399-2007
The detection method of coloration are as follows: GB11903-1989
The detection method of alcohols are as follows: HJ 895-2017
The detection method of organic acid are as follows: NB/T 12004-2016
The detection method of aniline are as follows: GB11889-1989
Embodiment 1
The processing method of a kind of synthesizing substituted and imidazoles organic wastewater, includes the following steps:
S1. waste water is distilled, is obtained containing 50% methanol, fraction is again through the methanol in rectifying recycling waste water；
S2. remaining mother liquor filtering, filtrate sulphur acid for adjusting pH to 3 are added 2g/L salting-out agents sodium sulphate, separate after distilling
Upper layer caprylic acid recycles the caprylic acid in waste water；
S3. lower aqueous layer sodium hydroxide adjusts pH value to 10, and the imitative extraction of chlorination separates chloroform layer, is evaporated under reduced pressure, is precipitated
O-phenylenediamine recycles the o-phenylenediamine in waste water；
S4. the organic matter in residual waste solution uses Fenton process deep oxidation, is adjusted with acid pH to 3 or so, and 3g/L is added
FeSO4·7H2O, 30mL/L 30%H2O2, maintain 40 DEG C of reaction 2h.CaO is added and adjusts pH value of solution to 9 or so, adds 1g/L
0.5g/L flocculation aid 0.1%PAM aqueous solution is added in flocculant 1%PAC aqueous solution, and flocculation sedimentation takes supernatant liquor, finally plus
Enter 3g/L active carbon decolorization adsorption, activated carbon particle size is 200 mesh.
The COD value of waste water is greatly reduced, and meets downstream garden sewage treatment plant adapter tube standard (≤500mg/L).
Embodiment 2
The processing method of a kind of synthesizing substituted and imidazoles organic wastewater, includes the following steps:
S1. waste water is distilled, is obtained containing 50% ethyl alcohol, fraction is again through the ethyl alcohol in rectifying recycling waste water；
S2. remaining mother liquor filtering, filtrate nitre acid for adjusting pH to 4 are added 3g/L salting-out agents potassium sulfate, separate after distilling
Upper layer n-caproic acid recycles the n-caproic acid in waste water；
S3. lower aqueous layer potassium hydroxide adjusting pH value to 11, the imitative extraction of chlorination, separates lower layer's chloroform layer, is evaporated under reduced pressure,
Aniline is precipitated, recycles the aniline in waste water；
S4. the organic matter in residual waste solution uses Fenton process deep oxidation, is adjusted with acid pH to 5 or so, and 4g/L is added
FeSO4·7H2O, 40mL/L 30%H2O2, maintain 50 DEG C of reaction 2h.CaO is added and adjusts pH value of solution to 7 or so, adds
0.5g/L flocculation aid 0.3%PAM aqueous solution is added in 0.5g/L flocculant 2%PAC aqueous solution, and flocculation sedimentation takes supernatant liquor,
It is eventually adding 4g/L active carbon decolorization adsorption, activated carbon particle size is 100 mesh.
The COD value of waste water is greatly reduced, and meets downstream garden sewage treatment plant adapter tube standard (≤500mg/L).
Embodiment 3
The processing method of a kind of synthesizing substituted and imidazoles organic wastewater, includes the following steps:
S1. waste water is distilled, is obtained containing 60% isopropanol, fraction is again through the isopropanol in rectifying recycling waste water；
S2. remaining mother liquor filtering, filtrate salt acid for adjusting pH to 3 are added 2g/L salting-out agents ammonium sulfate, separate after distilling
The positive valeric acid in upper layer recycles the positive valeric acid in waste water；
S3. lower aqueous layer potassium hydroxide adjusting pH value to 12, the imitative extraction of chlorination, separates lower layer's chloroform layer, is evaporated under reduced pressure,
M-phenylene diamine (MPD) is precipitated, recycles the m-phenylene diamine (MPD) in waste water；
S4. the organic matter in residual waste solution uses Fenton process deep oxidation, is adjusted with acid pH to 4 or so, and 5g/L is added
FeSO4·7H2O, 50mL/L 30%H2O2, maintain 40 DEG C of reaction 1h.CaO is added and adjusts pH value of solution to 8 or so, adds 2g/L
Flocculant 1%PAC aqueous solution, is added 1g/L flocculation aid 0.5%PAM aqueous solution, and flocculation sedimentation takes supernatant liquor, is eventually adding
5g/L active carbon decolorization adsorption, activated carbon particle size are 300 mesh.
The COD value of waste water is greatly reduced, and meets downstream garden sewage treatment plant adapter tube standard (≤500mg/L).
Embodiment 4
The processing method of a kind of synthesizing substituted and imidazoles organic wastewater, includes the following steps:
S1. waste water is distilled, is obtained containing 60% methanol, fraction is again through the methanol in rectifying recycling waste water；
S2. remaining mother liquor filtering, filtrate salt acid for adjusting pH to 5 are added 3g/L salting-out agents sodium sulphate, separate after distilling
The positive enanthic acid in upper layer recycles the positive enanthic acid in waste water；
S3. lower aqueous layer potassium hydroxide adjusting pH value to 11, the imitative extraction of chlorination, separates lower layer's chloroform layer, is evaporated under reduced pressure,
P-phenylenediamine is precipitated, recycles the p-phenylenediamine in waste water；
S4. the organic matter in residual waste solution uses Fenton process deep oxidation, is adjusted with acid pH to 4 or so, and 4g/L is added
FeSO4·7H2O, 40mL/L 30%H2O2, maintain 45 DEG C of reaction 2h.CaO is added and adjusts pH value of solution to 8 or so, adds
1.5g/L flocculation aid 0.4%PAM aqueous solution is added in 1.5g/L flocculant 2%PAC aqueous solution, and flocculation sedimentation takes supernatant liquor,
It is eventually adding 2g/L active carbon decolorization adsorption, activated carbon particle size is 200 mesh.
The COD value of waste water is greatly reduced, and meets downstream garden sewage treatment plant adapter tube standard (≤500mg/L).
Comparative example 1
The processing method of a kind of synthesizing substituted and imidazoles organic wastewater includes the following steps: using Fenton process depth
4g/L FeSO is added in oxidation4·7H2O, 40mL/L 30%H2O2, maintain 45 DEG C of reaction 2h.CaO is added and adjusts pH value of solution to 8
Left and right, adds 1.5g/L flocculant 2%PAC aqueous solution, is added 1.5g/L flocculation aid 0.4%PAM aqueous solution, flocculation sedimentation,
Supernatant liquor is taken, 2g/L active carbon decolorization adsorption is eventually adding, activated carbon particle size is 200 mesh.
As a result it detects
The result of the wastewater treatment of embodiment and comparative example is detected, detection data is as shown in table 2:
Table 2
| Serial number | The alcohols rate of recovery/% | Organic acid recovering rate/% | Aniline recovery rate/% | COD | Coloration |
| Embodiment 1 | 100 | 95 | 90 | 360 | 25 |
| Embodiment 2 | 100 | 96 | 92 | 185 | 16 |
| Embodiment 3 | 100 | 95 | 93 | 90 | 10 |
| Embodiment 4 | 100 | 96 | 92 | 400 | 31 |
| Comparative example 1 | 0 | 0 | 0 | 300000 | 168 |
As can be seen from the above Table 2, the organic wastewater obtained relative to existing Fenton process, processing method of the invention
COD value and coloration are substantially lower than comparative example 1, and the alcohols rate of recovery of waste water that processing method of the invention obtains can achieve
100%, the rate of recovery of organic acid also 95% or more, the rate of recovery of aniline also 90% or more, related Fenton rule entirely without
Method realizes the recycling of related waste water debirs.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all this
Made any modifications, equivalent replacements, and improvements etc., should be included in the claims in the present invention within the spirit and principle of invention
Protection scope within.
Claims (10)
1. a kind of processing method of synthesizing substituted and imidazoles organic wastewater, which comprises the steps of:
S1. the alcohols material in organic wastewater is separated and recovered, pure and mild recycling mother liquor is obtained；
S2. the recycling mother liquor in S1 is further separated and recovered into organic acid, obtains organic acid and recycling mother liquor；
S3. the recycling mother liquor in S2 is further separated and recovered into aniline, obtains aniline and separation waste liquid；
S4. the separation waste liquid Fenton process deep oxidation in S3 is flocculated, separates supernatant, sewage is sent in water outlet after decolorization adsorption removal
Treatment plant.
2. processing method as described in claim 1, which is characterized in that the separation and recovery method of alcohols material described in S1 are as follows: will
Organic wastewater distills to obtain the fraction containing 50~60% alcohols, and fraction is again through the alcohols material in rectifying recycling waste water.
3. processing method as described in claim 1, which is characterized in that separate and recover the method for organic acid described in S2 are as follows: by S1
In recycling mother liquor adjust pH to 3~6, salting-out agents are added, separate upper layer organic acid, recycle the organic acid in waste water.
4. processing method as described in claim 1, which is characterized in that separate and recover the method for aniline described in S3 are as follows: will be in S2
Recycling mother liquor adjust pH value to 9~12, add extractant to extract, aniline is precipitated in separating and extracting layer, vacuum distillation, recycles waste water
In aniline.
5. the processing method as described in Claims 1 to 4 any one, which is characterized in that the wadding of Fenton process deep oxidation described in S4
Solidifying concrete operations are as follows: the pH value for adjusting separation waste liquid is 2~5, and FeSO is added4·7H2O and H2O2Deep oxidation residual waste solution
In hard-degraded substance, adjusting pH value is 7~9, and flocculant and flocculation aid, flocculation sedimentation is added.
6. processing method as claimed in claim 5, which is characterized in that the FeSO4·7H2The additional amount of O is 3~5g/L, H2O2
For 30%H2O2, additional amount is 30~50mL/L.
7. processing method as claimed in claim 6, which is characterized in that the reaction temperature of the Fenton process deep oxidation is 35~50
DEG C, 1~2h of reaction time.
8. processing method as claimed in claim 5, which is characterized in that flocculant is the flocculant that mass fraction is 1%~3%
PAC aqueous solution, flocculation aid is the PAM aqueous solution that mass fraction is 0.1%~0.5%, on the basis of the volume of waste liquid.
9. processing method as claimed in claim 8, which is characterized in that the additive amount of flocculant PAC aqueous solution is 0.5~2g/L,
The additional amount of flocculation aid PAM aqueous solution is 0.5~4g/L.
10. processing method as claimed in claim 5, which is characterized in that decolorization adsorption is active carbon decolorization adsorption, activated carbon particle size
For 100~300 mesh, active carbon additional amount is 1~5g/L.
Priority Applications (1)
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| CN113045047A (en) * | 2021-03-29 | 2021-06-29 | 江西清绿环保有限公司 | Paint spraying wastewater purification and circulation system |
| CN114933390A (en) * | 2022-06-02 | 2022-08-23 | 扬州联博药业有限公司 | Method for treating aniline-containing wastewater generated in doxycycline hydrochloride production |
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