CN108569737A - The wastewater treatment method of the antifebrin route of para-ester - Google Patents
The wastewater treatment method of the antifebrin route of para-ester Download PDFInfo
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- CN108569737A CN108569737A CN201810365296.5A CN201810365296A CN108569737A CN 108569737 A CN108569737 A CN 108569737A CN 201810365296 A CN201810365296 A CN 201810365296A CN 108569737 A CN108569737 A CN 108569737A
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- waste water
- evaporation tubes
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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
- C02F1/043—Details
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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
- C02F1/34—Treatment of water, waste water, or sewage with mechanical oscillations
- C02F1/36—Treatment of water, waste water, or sewage with mechanical oscillations ultrasonic vibrations
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
- C07C303/04—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups
- C07C303/08—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups by reaction with halogenosulfonic acids
-
- 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
-
- 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
- C02F2301/06—Pressure conditions
- C02F2301/063—Underpressure, vacuum
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
Abstract
The wastewater treatment method of the antifebrin route of para-ester, belongs to para-ester field of waste water treatment.This method is used to handle chlorosulfonation waste water, including：Chlorosulfonation waste water is concentrated：Chlorosulfonation waste water is instilled by several droppers at the top of evaporation tubes, several heating rings are arranged side by side in evaporation tubes from the top to the bottom, the heating temperature of control heating ring is 95 120 DEG C, on the top of evaporation tubes, pumping makes the pressure in evaporation tubes remain 0.6 0.8atm, and the liquid for collecting instillation evaporation tubes bottom obtains Waste water concentrating liquid.And Waste water concentrating liquid and aniline reaction are obtained into p-aminobenzene sulfonic acid.It is simple for process, treatment effeciency is high, to comprehensive utilization of resources.
Description
Technical field
The present invention relates to para-ester field of waste water treatment, and the waste water of the antifebrin route of more particularly to a kind of para-ester
Processing method.
Background technology
Para-ester, alias is to beta-sulfuric ester ethyl sulfonyl aniline, ethylene sulfone sulfate, 4- ethyl-sulfate sulfuryl aniline, p- β-
Hydroxyl second sulfone aniline sulfuric ester, p- beta-hydroxy second sulfone aniline sulfuric ester.Para-ester is the important intermediate of reactive dye, is used for
Synthesize the reactive dye of fundamental mode containing vinyl sulfone(RemzaolHuo Xingranliaohuoxingjituan) such as EF types, KN types, M/KM types, ME types.
Para-ester is temporary water soluble group, is contained when can not only improve solubility when application, and dye
The reactive dye of hydroxyethyl sulfone sulfate base are low to fiber affinity, after some time it is possible to reach the effect of level dyeing is generated with fibration and contaminated
Material-fiber ehter bond, ehter bond acid resistance and thermal stability are good, are conducive to the wet fastness for improving detersive efficiency and dyeing and printing products.
At present in the synthetic method of para-ester, antifebrin is high as the maturity of Material synthesis para-ester, is a kind of master
The synthetic route wanted.But since the chlorosulphonation step of antifebrin route is balanced reaction, must be used greatly to improve yield just
The excessive chlorosulfonic acid of amount participates in reaction, produces a large amount of sulfuric acid wastewater containings.A kind of effective wastewater treatment method is studied for para-ester
The synthesis of antifebrin route be of great significance.
In view of this, special propose the application.
Invention content
The purpose of the present invention is to provide a kind of wastewater treatment method of the antifebrin route of para-ester, simple for process,
Treatment effeciency is high, to comprehensive utilization of resources.
The present invention solves its technical problem using following technical scheme to realize.
The present invention proposes a kind of wastewater treatment method of the antifebrin route of para-ester, for being carried out to chlorosulfonation waste water
Processing, including：
Chlorosulfonation waste water is concentrated：Chlorosulfonation waste water is instilled by several droppers at the top of evaporation tubes, evaporation
Several heating rings are arranged side by side in pipeline from the top to the bottom, and the heating temperature of control heating ring is 95-120 DEG C, in evaporation tubes
Top pumping so that the pressure in evaporation tubes is remained 0.6-0.8atm, collect and instill the liquid of evaporation tubes bottom and given up
Concentrated liquid.
And Waste water concentrating liquid and aniline reaction are obtained into p-aminobenzene sulfonic acid.
The advantageous effect of the embodiment of the present invention is：
Chlorosulfonation waste water is passed through several drops by the wastewater treatment method of the antifebrin route of para-ester provided by the invention
Pipe is entered in a manner of instilling in evaporation tubes, exhausted water drop in constantly fall during by heat ring heat effect not
Disconnected heating makes most of moisture be evaporated the remaining liquid phase being concentrated and instills evaporation tubes bottom.It is steamed as unit of drop
Hair, surface area increase, and disengagement area increases, and heating effect is good, are conducive to improve evaporation rate.It is taken out on top in heating process
Gas, on the one hand reduce pressure can reduce boiling point improve the efficiency of heating surface, on the other hand can promote evaporation moisture rapidly from
Discharge in evaporation tubes.Waste water concentrating liquid obtains p-aminobenzene sulfonic acid with aniline reaction, fully utilizes the sour conduct in waste water
Raw material；It is identical as main organic components in para-ester acid waste water to handle obtained p-aminobenzene sulfonic acid, can prepare high-purity
Spend product, non-secondary pollution.
Specific implementation mode
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, builds according to normal condition or manufacturer
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
The wastewater treatment method of the antifebrin route of the para-ester of the embodiment of the present invention is specifically described below.
The present invention provides a kind of wastewater treatment method of the antifebrin route of para-ester, for being carried out to chlorosulfonation waste water
Processing, including chlorosulfonation waste water is concentrated to give Waste water concentrating liquid, Waste water concentrating liquid and aniline reaction are obtained to amino
Benzene sulfonic acid.
Include specifically by the operation that chlorosulfonation waste water concentrates：By chlorosulfonation waste water by several droppers from evaporation tube
It is instilled at the top of road.The evaporation tubes have a tube wall in the setting of roughly vertical shape, and the inner walls of evaporation tubes is from the top to the bottom simultaneously
Row is provided with multiple heating rings.
The heating temperature of control heating ring is that the 95-120 DEG C of drop to instilling the chlorosulfonation waste water in evaporation tubes carries out
Heating evaporation, in some of the invention specific embodiments, heating degree be optionally 95 DEG C, 98 DEG C, 100 DEG C, 102 DEG C, 105
DEG C, 108 DEG C, 110 DEG C, 112 DEG C, 115 DEG C, 118 DEG C, 120 DEG C etc..
It is evaporated as unit of drop, surface area increases, and disengagement area increases, and heating effect is good, is conducive to improve and steam
Send out rate.
Preferably, before chlorosulfonation waste water is instilled evaporation tubes, it is pre- to being carried out in evaporation tubes with heating ring in advance
Heat can fully heat it just to start the when of instilling the drop of chlorosulfonation waste water, improve the evaporation effect of operation early period
Rate and evaporation effect.
During heating evaporation, on the top of evaporation tubes, pumping makes the pressure in evaporation tubes remain 0.6-
0.8atm, such as make pressure remain 0.6atm, 0.62atm, 0.65atm, 0.68atm, 0.7atm, 0.72atm, 0.75atm,
0.78atm, 0.8atm etc..
It is evacuated on top in heating process, on the one hand, the effect that boiling point improves heating evaporation moisture can be reduced by reducing pressure
Rate；On the other hand, the moisture evaporated can be promoted rapidly to be discharged from the top of evaporation tubes.
In some preferred embodiments of the invention, when the drop to chlorosulfonation waste water carries out heating evaporation, further include
To being ultrasonically treated in evaporation tubes.Specifically, such as can apply ultrasonic field to evaporation tubes to realize.
Preferably, be ultrasonically treated frequency be 1.2-2.0MHz, such as can be 1.2MHz, 1.3MHz, 1.4MHz,
1.5MHz, 1.6MHz, 1.7MHz, 1.8MHz, 1.9MHz, 2.0MHz etc..
To being ultrasonically treated in evaporation tubes, there is ultrasonication to the drop of the chlorosulfonation waste water in evaporation tubes
Effect, further increases the disengagement area of liquid, is conducive to further increasing for evaporation rate.
Further, when the drop to chlorosulfonation waste water carries out heating evaporation, hot sky is filled with to the bottom end of evaporation tubes
Gas, hot-air own vol, which expands, adds tip motions of the air-extraction function to evaporative light end, to chlorosulfonation waste water in motion process
Drop carry out more fully heating evaporation, while accelerating the vapor of evaporation evaporation tubes are discharged.
The present invention some specifically in embodiment, in order to improve the effect of logical hot-air：The temperature for the hot-air being passed through
Degree is 110-130 DEG C, such as can be 110 DEG C, 115 DEG C, 120 DEG C, 125 DEG C, 130 DEG C；Hot-air is filled in evaporation tubes
Initial velocity is 2-5cm/s, such as 2cm/s, 3cm/s, 4cm/s, 5cm/s.
Obtained Waste water concentrating liquid and aniline reaction are obtained into p-aminobenzene sulfonic acid, fully utilize the sour conduct in waste water
Raw material realizes the recycling to resource, preserves the ecological environment.Handle obtained p-aminobenzene sulfonic acid and para-ester acid waste water
In main organic components it is identical, high purity product, non-secondary pollution can be prepared.
Chlorosulfonation waste water is concentrated using above-mentioned method for concentration, the acidity of waste water greatly improves, and makes concentration waste water
It is improved with the reaction efficiency of aniline.The method for concentration is simple for process, and evaporation and concentration is compared with using conventional container for evaporation processing
Efficiency greatly improve.
Include specifically by the operation of Waste water concentrating liquid and aniline reaction：After Waste water concentrating liquid is heated, aniline is added dropwise
Into concentrating spent liquor.The mass ratio of Waste water concentrating liquid and aniline is preferably 4-6:1, such as 4:1、4.5:1、5:1、5.5:1、6:1
Deng, make raw material have higher utilization rate.
Waste water concentrating liquid is heated preferably to 80-120 DEG C, such as 80 DEG C, 85 DEG C, 90 DEG C, 95 DEG C, 100 DEG C, 105 DEG C, 110
DEG C, 115 DEG C, 120 DEG C etc..
The speed that aniline is added dropwise is unsuitable too fast, keeps substantially constant rate of addition, time for adding preferable during being added dropwise
Ground is 140-160min, as 140min, 142min, 145min, 148min, 150min, 152min, 155min, 158min,
160min etc..
In order to improve the reaction efficiency of Waste water concentrating liquid and aniline, preferably reaction solution is risen after dripping aniline
Temperature, temperature is preferably 180-190 DEG C after heating, such as 180 DEG C, 182 DEG C, 185 DEG C, 188 DEG C, 190 DEG C.
The reaction system of Waste water concentrating liquid and aniline reaction obtains crude product p-aminophenyl sulphur at being dried after fuse salt
Acid.
Further, high purity product in order to obtain, can also refine crude product p-aminobenzene sulfonic acid.
In carrying out some refined specific implementation modes to crude product p-aminobenzene sulfonic acid, including：Add water to dissolve by heating, adds
Adsorbent, filtering, condensing crystallizing.The temperature of heating for dissolving is 60-100 DEG C, more preferably 90-100 DEG C.Adsorbent is selected from activity
It is one or more in charcoal, diatomite, bentonite.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
A kind of wastewater treatment method of the antifebrin route of para-ester, including：
By the roughly vertical setting of evaporation tubes, 8 heating rings are arranged side by side from the top to the bottom in its inner wall.Control heating
Ring heating temperature is 95-100 DEG C of preheating 30-45min, and 5L chlorosulfonations waste water is dripped by 40 droppers from the top of evaporation tubes
Enter, 120-130 DEG C of hot-air is passed through to evaporation tubes bottom with the initial velocity of 2cm/s while instillation, with 1.2-2.0MHz
Frequency to being ultrasonically treated in evaporation tubes, while the top of evaporation tubes pumping so that the pressure in evaporation tubes is kept
For 0.6-0.7atm.The liquid for instilling evaporation tubes bottom is collected, the Waste water concentrating liquid that acidity is 73.6% is obtained.
It is 6 according to the mass ratio of Waste water concentrating liquid and aniline:1 prepares aniline raw material.Waste water concentrating liquid is heated to 100-
After 120 DEG C, aniline is instilled into Waste water concentrating liquid with slow uniform speed in 150-160min.Reaction solution is heated to 180-
190 DEG C to reactant at fuse salt state, be dried to obtain crude product p-aminobenzene sulfonic acid.
Embodiment 2
A kind of wastewater treatment method of the antifebrin route of para-ester, including：
By the roughly vertical setting of evaporation tubes, 6 heating rings are arranged side by side from the top to the bottom in its inner wall.Control heating
Ring heating temperature is 100-110 DEG C of preheating 30-45min, by 5L chlorosulfonations waste water by 48 droppers from the top of evaporation tubes
It instills, 110-120 DEG C of hot-air is passed through to evaporation tubes bottom with the initial velocity of 3cm/s while instillation, with 1.2-
To being ultrasonically treated in evaporation tubes, while at the top of evaporation tubes, pumping makes the pressure in evaporation tubes to the frequency of 2.0MHz
Remain 0.6-0.7atm by force.The liquid for instilling evaporation tubes bottom is collected, the Waste water concentrating liquid that acidity is 75.1% is obtained.
It is 5.5 according to the mass ratio of Waste water concentrating liquid and aniline:1 prepares aniline raw material.Waste water concentrating liquid is heated to 80-
After 100 DEG C, aniline is instilled into Waste water concentrating liquid with slow uniform speed in 140-150min.Reaction solution is heated to 180-
190 DEG C to reactant at fuse salt state, be dried to obtain crude product p-aminobenzene sulfonic acid.
Embodiment 3
A kind of wastewater treatment method of the antifebrin route of para-ester, including：
By the roughly vertical setting of evaporation tubes, 6 heating rings are arranged side by side from the top to the bottom in its inner wall.Control heating
Ring heating temperature is 110-120 DEG C of preheating 30-45min, by 5L chlorosulfonations waste water by 52 droppers from the top of evaporation tubes
It instills, 120-130 DEG C of hot-air is passed through to evaporation tubes bottom with the initial velocity of 4cm/s while instillation, with 1.2-
To being ultrasonically treated in evaporation tubes, while at the top of evaporation tubes, pumping makes the pressure in evaporation tubes to the frequency of 2.0MHz
Remain 0.6-0.7atm by force.The liquid for instilling evaporation tubes bottom is collected, the Waste water concentrating liquid that acidity is 75.8% is obtained.
It is 5 according to the mass ratio of Waste water concentrating liquid and aniline:1 prepares aniline raw material.Waste water concentrating liquid is heated to 100-
After 120 DEG C, aniline is instilled into Waste water concentrating liquid with slow uniform speed in 150-160min.Reaction solution is heated to 180-
190 DEG C to reactant at fuse salt state, be dried to obtain crude product p-aminobenzene sulfonic acid.
Embodiment 4
A kind of wastewater treatment method of the antifebrin route of para-ester, including：
By the roughly vertical setting of evaporation tubes, 6 heating rings are arranged side by side from the top to the bottom in its inner wall.Control heating
Ring heating temperature is 110-120 DEG C of preheating 30-45min, by 5L chlorosulfonations waste water by 60 droppers from the top of evaporation tubes
It instills, 120-130 DEG C of hot-air is passed through to evaporation tubes bottom with the initial velocity of 5cm/s while instillation, with 1.2-
To being ultrasonically treated in evaporation tubes, while at the top of evaporation tubes, pumping makes the pressure in evaporation tubes to the frequency of 2.0MHz
Remain 0.7-0.8atm by force.The liquid for instilling evaporation tubes bottom is collected, the Waste water concentrating liquid that acidity is 77.3% is obtained.
It is 4 according to the mass ratio of Waste water concentrating liquid and aniline:1 prepares aniline raw material.Waste water concentrating liquid is heated to 100-
After 120 DEG C, aniline is instilled into Waste water concentrating liquid with slow uniform speed in 150-160min.Reaction solution is heated to 180-
190 DEG C to reactant at fuse salt state, be dried to obtain crude product p-aminobenzene sulfonic acid.
Comparative example
A kind of wastewater treatment method of the antifebrin route of para-ester, with embodiment 4 the difference is that：Using
Distillation under vacuum, by chlorosulfonation Waste water concentrating to acid under conditions of pressure is 110-120 DEG C of 0.7-0.8atm and heating temperature
Degree about 75%.
After tested, the consumption of the wastewater treatment method of the antifebrin route for the para-ester that embodiment 1-4 and comparative example 1 provide
It can be quite.The concentration operation of embodiment 1-4 takes compared with the concentration operation of comparative example shortens about 10-20%.
In conclusion the wastewater treatment method of the antifebrin route of para-ester provided by the invention, as unit of drop
It is evaporated, surface area increases, and disengagement area increases, and heating effect is good, is conducive to improve evaporation rate.It is being pushed up in heating process
End pumping, the boiling point raising efficiency of heating surface can be reduced by the one hand reducing pressure, and the moisture of evaporation on the other hand can be promoted quick
Ground is discharged out of evaporation tubes.Waste water concentrating liquid obtains p-aminobenzene sulfonic acid with aniline reaction, fully utilizes the acid in waste water
As raw material；It is identical as main organic components in para-ester acid waste water to handle obtained p-aminobenzene sulfonic acid, can prepare
High purity product, non-secondary pollution.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of wastewater treatment method of the antifebrin route of para-ester, for handling chlorosulfonation waste water, feature
It is, including：
The chlorosulfonation waste water is concentrated：The chlorosulfonation waste water is instilled by several droppers at the top of evaporation tubes,
Several heating rings are arranged side by side in the evaporation tubes from the top to the bottom, and the heating temperature for controlling the heating ring is 95-120
DEG C, on the top of the evaporation tubes, pumping makes the pressure in the evaporation tubes remain 0.6-0.8atm, collects and instills institute
The liquid for stating evaporation tubes bottom obtains Waste water concentrating liquid；And
The Waste water concentrating liquid and aniline reaction are obtained into p-aminobenzene sulfonic acid.
2. wastewater treatment method according to claim 1, which is characterized in that the behaviour for concentrating the chlorosulfonation waste water
Work further includes：To being ultrasonically treated in the evaporation tubes.
3. wastewater treatment method according to claim 2, which is characterized in that the frequency of supersound process is 1.2-2.0MHz.
4. wastewater treatment method according to claim 1, which is characterized in that the behaviour for concentrating the chlorosulfonation waste water
Work further includes：It is filled with hot-air to the bottom end of the evaporation tubes.
5. wastewater treatment method according to claim 4, which is characterized in that the temperature of the hot-air is 110-130 DEG C；
And/or it is 2-5cm/s that the hot-air, which is filled with the initial velocity in the evaporation tubes,.
6. according to claim 1-5 any one of them wastewater treatment methods, which is characterized in that the Waste water concentrating liquid with it is described
The mass ratio of aniline is 4-6:1.
7. wastewater treatment method according to claim 6, which is characterized in that the Waste water concentrating liquid and the aniline is anti-
The operation answered includes：After the Waste water concentrating liquid is heated to 80-120 DEG C, the aniline is added dropwise to the Waste water concentrating liquid.
8. wastewater treatment method according to claim 7, which is characterized in that the time for adding of the aniline is 140-
160min。
9. wastewater treatment method according to claim 7, which is characterized in that the Waste water concentrating liquid is anti-with the aniline
It is 180-190 DEG C to answer temperature.
10. wastewater treatment method according to claim 1, which is characterized in that further include to the p-aminobenzene sulfonic acid into
Row is refined.
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| CN201810365296.5A CN108569737A (en) | 2018-04-23 | 2018-04-23 | The wastewater treatment method of the antifebrin route of para-ester |
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| CN201810365296.5A CN108569737A (en) | 2018-04-23 | 2018-04-23 | The wastewater treatment method of the antifebrin route of para-ester |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109912463A (en) * | 2019-04-10 | 2019-06-21 | 新乡市锦源化工有限公司 | A kind of contraposition Lipase absobed and wastewater treatment method |
| CN110117118A (en) * | 2019-04-26 | 2019-08-13 | 浙江龙盛化工研究有限公司 | A kind of processing method of chlorosulfonation acid waste water |
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| CN110117118A (en) * | 2019-04-26 | 2019-08-13 | 浙江龙盛化工研究有限公司 | A kind of processing method of chlorosulfonation acid waste water |
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Application publication date: 20180925 |