CN108129271A - A kind of method of the chloro- 3,5- dinitro-p-trifluorotoluenes waste water acidification recycling phenol of 4- - Google Patents
A kind of method of the chloro- 3,5- dinitro-p-trifluorotoluenes waste water acidification recycling phenol of 4- Download PDFInfo
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- CN108129271A CN108129271A CN201810017404.XA CN201810017404A CN108129271A CN 108129271 A CN108129271 A CN 108129271A CN 201810017404 A CN201810017404 A CN 201810017404A CN 108129271 A CN108129271 A CN 108129271A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/685—Processes comprising at least two steps in series
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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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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
- C07C37/72—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by liquid-liquid treatment
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
- C07C37/82—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by solid-liquid treatment; by chemisorption
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/86—Purification; separation; Use of additives, e.g. for stabilisation by treatment giving rise to a chemical modification
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- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- 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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
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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
- C02F2303/00—Specific treatment goals
- C02F2303/16—Regeneration of sorbents, filters
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- 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
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Abstract
The present invention relates to a kind of methods of 4 chlorine 3,5 dinitro-p-trifluorotoluene waste water acidification recycling phenol, include the following steps：S1 is acidified；S2 is filtered：By mixed liquor in S1 steps using plate-frame filtering, solid is dried；S3 is adsorbed：Resin is added in filter, then the filtrate in S2 steps is added in into adsorption filtration in filter with the rate of 1.0 2.0ml/min, filtrate is transferred to sewage plant carries out biochemical treatment；S4 regenerates：Lye is added in resin into S3 steps for regenerating resin, obtains regenerated liquid；S5 is recycled：Inorganic acid II is added in regenerated liquid into S4 steps and adjusts PH to 57, adds in organic solvent extraction, solvent flashing obtains phenol.The present invention has the advantages that at low cost, regeneration efficiency is high and purity is high.
Description
Technical field
The present invention relates to technical field of waste water processing, and in particular to a kind of chloro- 3,5- dinitro-p-trifluorotoluenes waste water acid of 4-
Change the method for recycling phenol.
Background technology
With the fast development of China's economy, organic nitrification industry also emerges rapidly, and nitrobenzene, which is important, to become more meticulous
Work intermediate, but nitration processes are inevitably generated a large amount of nitration waste water, and nitre is further included other than spent acid in waste water
Change the substances such as product and nitropheneol, have the toxicity big, it is difficult to which the features such as biochemical treatment, the processing of nitration waste water is still at waste water
The problem of reason.
Chloro- 3, the 5- dinitro-p-trifluorotoluenes intermediate products of Products 4-, the material (abbreviation itrated compound) point after nitrification are gone
It needs to wash material after nitration mixture layer and alkali cleaning, at this time waste water of the generation with itrated compound, 5 tons of itrated compound generation per ton is given up
Water.Since waste water is handed in buff and toxicity big, sewage plant processing cannot be introduced into, it is necessary to which the waste water is pre-processed.Tradition
Pretreating process uses activated carbon adsorption bleaching three times, can be only achieved into sewage plant processing requirement, but activated carbon usage amount reaches
To 50Kg/t waste water, and waste active carbon will become hazardous waste, need outer processing of entrusting, and disposition takes high.
This project is intended using the method for resin adsorption come Phenol-Containing Wastewater Treatment, using large aperture resin by itrated compound in waste water
Absorption, substantially reduces COD and phenols in nitration waste water, enters sewage plant water inlet index so as to reach, resin can be recycled and be followed
Ring uses.
Invention content
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of chloro- 3, the 5- dinitro-p-trifluorotoluenes of 4- to give up
The method of water acidification recycling phenol, solves the problems, such as that cost for wastewater treatment is high.
The purpose of the present invention is achieved through the following technical solutions：
A kind of method of chloro- 3, the 5- dinitro-p-trifluorotoluenes waste water acidification recycling phenol of 4-, includes the following steps：
S1 is acidified：By in the waste water input acid precipitation reaction kettle of chloro- 3, the 5- dinitro-p-trifluorotoluenes of 4-, adding in inorganic acid I will
PH is adjusted to 1-2, is stood 12-24h, is obtained mixed liquor；
S2 is filtered：By mixed liquor in S1 steps using plate-frame filtering, solid is dried；
S3 is adsorbed：Resin is added in filter, then the filtrate in S2 steps is added in the rate of 1.0-2.0ml/min
Filtrate is transferred to sewage plant and carries out biochemical treatment by adsorption filtration in filter；
S4 regenerates：Lye is added in resin into S3 steps for regenerating resin, obtains regenerated liquid；
S5 is recycled：Inorganic acid II is added in regenerated liquid into S4 steps and adjusts PH to 5-7, adds in organic solvent extraction,
Solvent flashing obtains phenol.
Resin is a kind of high molecular polymer to organic matter with concentration and separation effect, both with certain specific surface area
And pore, and there is various polarity and different function group, wherein chemisorbed plays particularly important effect；Utilize large aperture
Resin adsorbs itrated compound in waste water, substantially reduces COD and phenols in nitration waste water, refers to so as to reach into sewage plant water inlet
Mark, and resin can recycle.
Further, the inorganic acid I in the S1 steps is sulfuric acid or nitric acid.
Further, the hydrogen ion molar concentration of the inorganic acid I is 1-5mol/L.
Further, the resin is polar macroporous adsorption resin.The aperture of macroporous absorbent resin and specific surface area all compare
It is larger, inside resin there is three dimensions solid pore structure, there is physical and chemical stability height, large specific surface area, absorption to hold
Amount is big, selectivity is good, adsorption rate is fast, desorption condition is mild, regeneration treatment is convenient, service life is long, is suitable for composition is closed circuit to follow
Ring, many advantages, such as saving money.
Further, the resin and the mass ratio of filtrate are 1：20-50.
Further, the lye in the S4 steps is the sodium hydroxide solution of 0.95-1.05mol/L.
Further, the inorganic acid II in the S5 steps is the sulfuric acid or nitric acid of 0.01-0.05mol/L.
In acidization, adjusted using strong acid, be easy in the later stage remove and it is nontoxic, can be directly entered sewage plant into
Row biochemical treatment, lye selection highly basic, regeneration rate is fast, immiscible with organic solvent, conducive to later stage purification by liquid extraction.
Further, the organic solvent in the S5 steps is ether or dichloromethane.Organic solvent selection low boiling point is easy
Recovered solvent, and solubility is high.
The beneficial effects of the invention are as follows：
1. adsorbing itrated compound in waste water using large aperture resin, substantially reduce COD and phenols in nitration waste water, so as to
Reach into sewage plant water inlet index, resin can recycle；
2. resin is a kind of high molecular polymer to organic matter with concentration and separation effect, both with certain specific surface
Product and pore, and there is various polarity and different function group, wherein chemisorbed plays particularly important effect；
3. in acidization, adjusted using strong acid, be easy to remove in the later stage and nontoxic, sewage plant can be directly entered
Biochemical treatment is carried out, lye selection highly basic, regeneration rate is fast, immiscible with organic solvent, conducive to later stage purification by liquid extraction.
Specific embodiment
Technical scheme of the present invention is described in further detail, but protection scope of the present invention is not with reference to specific embodiment
It is confined to as described below.
A kind of method of chloro- 3, the 5- dinitro-p-trifluorotoluenes waste water acidification recycling phenol of 4-, includes the following steps：
S1 is acidified：By in the waste water input acid precipitation reaction kettle of chloro- 3, the 5- dinitro-p-trifluorotoluenes of 4-, adding in inorganic acid I will
PH is adjusted to 1-2, is stood 12-24h, is obtained mixed liquor；
S2 is filtered：By mixed liquor in S1 steps using plate-frame filtering, solid is dried；
S3 is adsorbed：Resin is added in filter, then the filtrate in S2 steps is added in the rate of 1.0-2.0ml/min
Filtrate is transferred to sewage plant and carries out biochemical treatment by adsorption filtration in filter；
S4 regenerates：Lye is added in resin into S3 steps for regenerating resin, obtains regenerated liquid；
S5 is recycled：Inorganic acid II is added in regenerated liquid into S4 steps and adjusts PH to 5-7, adds in organic solvent extraction,
Solvent flashing obtains phenol.
Specifically, the inorganic acid I in the S1 steps is sulfuric acid or nitric acid.
Specifically, the hydrogen ion molar concentration of the inorganic acid I is 1-5mol/L.
Specifically, the resin is polar macroporous adsorption resin.
Specifically, the resin and the mass ratio of filtrate are 1：20-50.
Specifically, the lye in the S4 steps is the sodium hydroxide solution of 0.95-1.05mol/L.
Specifically, the inorganic acid II in the S5 steps is the sulfuric acid or nitric acid of 0.01-0.05mol/L.
Specifically, the organic solvent in the S5 steps is ether or dichloromethane.
The specific implementation parameter of embodiment 1- embodiments 5 is as shown in table 1, and 4 present invention of embodiment 1- embodiments limits
The comparative examples of technical parameter, wherein embodiment 5 for the present invention, embodiment 5 are activated carbon adsorption bleaching three times.
Table 1
The handling result of embodiment 1 is as shown in table 2：
Table 2
The handling result of embodiment 2 is as shown in table 3：
| Project | COD(mg/L) | Nitrophenols (mg/L) | Coloration | Appearance |
| Raw water | 9660 | 600 | 3000 | Dark-brown |
| Acid is adjusted to cross drainage | 5480 | 460 | 500 | Brown color |
| Adsorb water | 1860 | It does not detect | 30 | It is near colourless |
Table 3
The handling result of embodiment 3 is as shown in table 4：
| Project | COD(mg/L) | Nitrophenols (mg/L) | Coloration | Appearance |
| Raw water | 9660 | 600 | 3000 | Dark-brown |
| Acid is adjusted to cross drainage | 5500 | 470 | 500 | Brown color |
| Adsorb water | 2150 | It does not detect | 30 | It is near colourless |
Table 4
The handling result of embodiment 4 is as shown in table 5：
| Project | COD(mg/L) | Nitrophenols (mg/L) | Coloration | Appearance |
| Raw water | 9660 | 600 | 3000 | Dark-brown |
| Acid is adjusted to cross drainage | 5480 | 460 | 500 | Brown color |
| Adsorb water | 2080 | It does not detect | 30 | It is near colourless |
Table 5
The handling result of embodiment 5 is as shown in table 6：
| Project | COD(mg/L) | Nitrophenols (mg/L) | Coloration | Appearance |
| Raw water | 9660 | 600 | 3000 | Dark-brown |
| Adsorb water | 2680 | It does not detect | 30 | It is near colourless |
Table 6
The above is only the preferred embodiment of the present invention, it should be understood that the present invention is not limited to described herein
Form is not to be taken as the exclusion to other embodiment, and available for other combinations, modifications, and environments, and can be at this
In the text contemplated scope, modifications can be made through the above teachings or related fields of technology or knowledge.And those skilled in the art institute into
Capable modifications and changes do not depart from the spirit and scope of the present invention, then all should be in the protection domain of appended claims of the present invention
It is interior.
Claims (8)
- A kind of 1. method of chloro- 3, the 5- dinitro-p-trifluorotoluenes waste water acidification recycling phenol of 4-, which is characterized in that including walking as follows Suddenly：S1 is acidified：By in the waste water input acid precipitation reaction kettle of chloro- 3, the 5- dinitro-p-trifluorotoluenes of 4-, inorganic acid I is added in by PH tune Section stands 12-24h, obtains mixed liquor to 1-2；S2 is filtered：By mixed liquor in S1 steps using plate-frame filtering, solid is dried；S3 is adsorbed：Resin is added in filter, then the filtrate in S2 steps is added in into filtering with the rate of 1.0-2.0ml/min Filtrate is transferred to sewage plant and carries out biochemical treatment by adsorption filtration in device；S4 regenerates：Lye is added in resin into S3 steps for regenerating resin, obtains regenerated liquid；S5 is recycled：Inorganic acid II is added in regenerated liquid into S4 steps and adjusts PH to 5-7, adds in organic solvent extraction, volatilization Solvent obtains phenol.
- 2. a kind of method of chloro- 3, the 5- dinitro-p-trifluorotoluenes waste water acidification recycling phenol of 4- according to claim 1, It is characterized in that, the inorganic acid I in the S1 steps is sulfuric acid or nitric acid.
- 3. a kind of side of the chloro- 3,5- dinitro-p-trifluorotoluenes waste water acidification recycling phenol of 4- according to claim 1 or 2 Method, which is characterized in that the hydrogen ion molar concentration of the inorganic acid I is 1-5mol/L.
- 4. a kind of method of chloro- 3, the 5- dinitro-p-trifluorotoluenes waste water acidification recycling phenol of 4- according to claim 1, It is characterized in that, the resin is polar macroporous adsorption resin.
- 5. a kind of side of the chloro- 3,5- dinitro-p-trifluorotoluenes waste water acidification recycling phenol of 4- according to claim 1 or 4 Method, which is characterized in that the resin and the mass ratio of filtrate are 1：20-50.
- 6. a kind of method of chloro- 3, the 5- dinitro-p-trifluorotoluenes waste water acidification recycling phenol of 4- according to claim 1, It is characterized in that, the lye in the S4 steps is the sodium hydroxide solution of 0.95-1.05mol/L.
- 7. a kind of method of chloro- 3, the 5- dinitro-p-trifluorotoluenes waste water acidification recycling phenol of 4- according to claim 1, It is characterized in that, the inorganic acid II in the S5 steps is the sulfuric acid or nitric acid of 0.01-0.05mol/L.
- 8. a kind of method of chloro- 3, the 5- dinitro-p-trifluorotoluenes waste water acidification recycling phenol of 4- according to claim 1, It is characterized in that, the organic solvent in the S5 steps is ether or dichloromethane.
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| CN201810017404.XA CN108129271A (en) | 2018-01-09 | 2018-01-09 | A kind of method of the chloro- 3,5- dinitro-p-trifluorotoluenes waste water acidification recycling phenol of 4- |
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| CN201810017404.XA CN108129271A (en) | 2018-01-09 | 2018-01-09 | A kind of method of the chloro- 3,5- dinitro-p-trifluorotoluenes waste water acidification recycling phenol of 4- |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115093041A (en) * | 2022-02-22 | 2022-09-23 | 邓国文 | Recycling treatment method for industrial wastewater generated by producing 5-amino-2-nitrobenzotrifluoride |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115093041A (en) * | 2022-02-22 | 2022-09-23 | 邓国文 | Recycling treatment method for industrial wastewater generated by producing 5-amino-2-nitrobenzotrifluoride |
| CN115093041B (en) * | 2022-02-22 | 2024-02-13 | 杨自林 | Recycling treatment method of industrial wastewater generated in production of 5-amino-2-nitrobenzotrifluoride |
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