CN110002656A - A kind of ethyl acetate liquid waste treatment system and its processing method - Google Patents

A kind of ethyl acetate liquid waste treatment system and its processing method Download PDF

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Publication number
CN110002656A
CN110002656A CN201910412360.5A CN201910412360A CN110002656A CN 110002656 A CN110002656 A CN 110002656A CN 201910412360 A CN201910412360 A CN 201910412360A CN 110002656 A CN110002656 A CN 110002656A
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solid
ice crystal
liquid
ice
separating
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CN201910412360.5A
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张乐华
周龙达
何旻绮
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Shanghai Shishi Hewei Chemical Industry Co Ltd
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Shanghai Shishi Hewei Chemical Industry Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00Multistage treatment of water, waste water or sewage
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/22Treatment of water, waste water, or sewage by freezing
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/24Treatment of water, waste water, or sewage by flotation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/38Treatment of water, waste water, or sewage by centrifugal separation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F7/00Aeration of stretches of water

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  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Physical Water Treatments (AREA)

Abstract

The invention discloses a kind of processing systems of ethyl acetate waste liquid, it is characterized in that, including consisting of part: air-floating apparatus, middle tank, the ice crystal crystallizer with slice ice machine, slaking reaction device, equipment for separating liquid from solid installed in order, wherein, the liquid separating opening of the equipment for separating liquid from solid is connected with the liquids recovery mouth of a recovery pond, and the liquid outlet opening of the recovery pond is connected with the ice crystal crystallizer;The solid separating opening of the equipment for separating liquid from solid is connected with a solid recovery unit;The ice crystal separating opening of the equipment for separating liquid from solid is connected with the ice crystal feed inlet of an ice water tank, and the ice crystal discharge port of the ice water tank is connected in the ice crystal crystallizer.The invention also discloses its processing methods.

Description

A kind of ethyl acetate liquid waste treatment system and its processing method
Technical field
The invention belongs to technical field of waste water processing, and in particular to a kind of processing system and its processing of ethyl acetate waste liquid Method
Background technique
Ethyl acetate is a kind of industrial chemicals that application is very wide, is a kind of quick-drying solvent, has excellent solvability, It can be widely applied to textile industry, food service industry and pharmaceutical industry.The extensive use of ethyl acetate drives upstream ethyl acetate The development of manufacturer can also generate a large amount of production of ethyl waste water at the same time, and ethyl acetate industrial wastewater is without place The problem of reason direct emission is brought is main, and there are two aspects: first is that the pollution to water environment.Ethyl acetate waste water has for high concentration Machine waste water, into water body after rapidly deplete dissolved oxygen in water body, and ethyl acetate is to the irritant effect of eye, nose, throat, Human body can generate some ill symptoms such as Nausea and vomiting, abdominal pain, diarrhea.If contacted for a long time, it is possible to will lead to people Body eye cornea is muddy, the secondary anemia of blood, leukocytosis, acute pulmonary edema, the illnesss such as liver, renal damage, additionally There is certain sensitization, bleeding gums, eczema-like dermatitis etc. can be caused.Second is that since ethyl acetate is volatile organic matter (VOC), steam is heavier than air, and quite remote place can be diffused into lower.Butanol vapor and air can form explosion Property mixture become chemical company's danger source.Therefore, it deals carefully with ethyl acetate waste water, realize wastewater zero discharge and recycling benefit With as current problem urgently to be resolved.
The technique of industrial processing ethyl acetate waste water there are several types of:
The way of distillation: the fresh water water quality that way of distillation processing waste water has easy to operate, simple process, processing to obtain is good etc. excellent Point.But there are still many disadvantages using way of distillation processing organic intermediate production waste water: the way of distillation is only applicable to laboratory at present And midget plant, it can not be mass produced;Actually and it can not be kept completely separate water and inorganic salts, main cause is the two The difference of relative volatility;Full-scale plant cost is high, is easy fouling, and energy consumption is high, it is virtually impossible to it gets a profit, it is undesirable.
Resin adsorption method: resin adsorption method has good treatment effect for organic intermediate production waste water, passes through selection Different types of resin and the polarity for improving resin, can be improved the selectivity and adsorption efficiency of resin.Certain absorption are polluted The resin of object can also recycle utility in waste water after carrying out desorption processing.But resin adsorption method also has insufficient place: resin Intensity difference, be easily damaged in use process, service life is short, causes operating cost higher;To high operation requirements, adsorbent Regeneration and update are difficult;Be not suitable for high throughput and the biggish scene of variation water quality.
Membrane separation process: using membrane separation process to handle organic intermediate and produce waste water, has and handles efficient, the low, energy consumption of pollution The advantages that low, recyclable pure water and useful component, processing equipment compact is easy to operate, easy to maintain.But how to produce honest and clean The service life problem of high performance selective membrane and film constrains the extensive use of membrane separation technique in the treatment of waste water to valence again.
Biochemical method: biological treatment is the most commonly used routine techniques of current waste water treatment applications, has processing cost low, suitable The advantages that wide, adaptable with range.But organic intermediate produces waste water since pollutant concentration is excessively high, and contains a large amount of nothing Machine salt substance has inhibition and toxic action to the growth of microorganism, cannot be had under normal circumstances using conventional biochemical method processing Machine intermediate produces waste water.
Ethyl acetate waste liquid belongs to high concentration, organic high-salinity wastewater, the conventional process waste water higher cost, and locates It is lower to manage efficiency.The salt utilized in the waste water containing a large amount of resourcebilities, wastewater treatment can be reduced by carrying out comprehensive utilzation to it Cost.
Summary of the invention
In order to overcome the drawbacks described above of the prior art, the purpose of the present invention is to provide a kind of processing of ethyl acetate waste liquid System and its processing method.
In order to achieve the object of the present invention, used technical solution is:
A kind of processing system of ethyl acetate waste liquid, including consisting of part:
Air-floating apparatus, middle tank, the ice crystal crystallizer with slice ice machine, slaking reaction device, solid-liquid installed in order Separator, wherein the liquid separating opening of the equipment for separating liquid from solid is connected with the liquids recovery mouth of a recovery pond, the recycling The liquid outlet opening in pond is connected with the ice crystal crystallizer;The solid separating opening of the equipment for separating liquid from solid and solid recycling fill It sets connected;The ice crystal separating opening of the equipment for separating liquid from solid is connected with the ice crystal feed inlet of an ice water tank, the ice of the ice water tank Brilliant discharge port is connected in the ice crystal crystallizer.
In a preferred embodiment of the invention, the slaking reaction device is that the ripening at low temperature with agitating device is anti- Answer device.
It in a preferred embodiment of the invention, include centrifugal separator in the equipment for separating liquid from solid.
In order to achieve the object of the present invention, used another solution is that
A kind of processing method of ethyl acetate waste liquid, includes the following steps:
The ethyl acetate waste liquid generated after production, which is pumped into air-floating apparatus, carries out aeration air bearing pretreatment, by being aerated air bearing Waste liquid afterwards is discharged into middle tank storage;
Periodically the waste liquid of storage is discharged into ice crystal crystallizer and carries out decrease temperature crystalline, slice ice machine smashes ice crystal, is crushed Ice crystal afterwards is passed through in slaking reaction device and carries out ripening at low temperature 4-8 hours;
Curing separation of the ice crystal through centrifuge in equipment for separating liquid from solid after primary curing, the equipment for separating liquid from solid will Filtrate and salinity separating and recovering in ice crystal, wherein filtrate is discharged into recovery pond, and solid salinity is discharged into solid recovery unit, Ice crystal after residue centrifugation is discharged into ice water tank;
Filtrate after collecting is recrystallized from being passed through again in ice crystal crystallizer in recovery pond, and after collecting Ice crystal carries out ripening at low temperature again after being discharged into slaking reaction device in ice water tank.
The beneficial effects of the present invention are:
The present invention not only realizes the purification of ethyl acetate waste liquid, can also recycle salinity simultaneously, realize wastewater zero discharge and Resource utilization achievees the purpose that environmental protection, has a vast market application prospect and economic benefit.
Detailed description of the invention
Fig. 1 is flow diagram of the invention.
Specific embodiment
The present invention is further illustrated below by specific embodiment and embodiment.
The processing system 1000 of a kind of ethyl acetate waste liquid as shown in Figure 1, including the air-floating apparatus installed in order 100, middle tank 200, the ice crystal crystallizer 300 with slice ice machine 310, the ripening at low temperature reactor 400 with blender 410 And have 510 equipment for separating liquid from solid 500 of centrifugal separator.
Wherein air-floating apparatus 100 passes through discharge port 102 and middle tank other than the feed inlet 101 with feed pump 110 200 water inlet 201 is connected, and the water outlet 202 of middle tank 200 is connected with the ice crystal import 301 of ice crystal crystallizer 300, ice The ice crystal outlet 302 of brilliant crystallizer 300 is connected with the curing import 401 of ripening at low temperature reactor 400, ripening at low temperature reactor 400 curing outlet 402 is connected with the separation import 501 of equipment for separating liquid from solid 500.
In equipment for separating liquid from solid 500, other than the separation import 501 being connected with ripening at low temperature reactor 400, also pass through Liquid separating opening 502 is connected with the liquids recovery mouth 601 of recovery pond 600;Pass through solid separating opening 503 and solid recovery unit 700 are connected;It is connected by ice crystal separating opening 504 with the ice water feed inlet 801 of ice water tank 800.
In order to further promote recycling and isolated degree, the liquid outlet opening 602 and ice crystal crystallizer of recovery pond 600 300 filtrate recovery port 303 is connected.The curing import of the ice water discharge port 802 and ripening at low temperature reactor 400 of ice water tank 800 403 are connected.
Due to using above-mentioned structure, the working principle of the invention is:
The waste liquid containing ethyl acetate and inorganic salts generated in industrial production is by the effect of feed pump 110 from feed inlet 101, which are pumped into progress air-dissolving air-float, the waste liquid after air-dissolving air-float in air-floating apparatus 100, is stored in middle tank 200.It is fixed Waste liquid after phase storage is pumped into ice crystal crystallizer 300 by the discharging pump 210 of middle tank 200 and carries out level-one freezing processing.
In ice crystal crystallizer 300, slice ice machine 310 by the ice crystal of bulk be broken into broken and tiny ice crystal it is broken after again will It is discharged into ripening at low temperature reactor 400, stirs ripening at low temperature 7 hours under the action of blender 410, and due to blender 410 effect, conducive to the initial gross separation of salt and ice crystal.Ice crystal crystallizer 300 is continuity or batch-type crystallizer, material therein Liquid temperature maintains between -15 DEG C to -20 DEG C.
Then the mixture after initial gross separation is passed through in equipment for separating liquid from solid 500, in the effect of centrifugal separator 510 Under, salt, ice crystal and filtrate in mixture are separated, and salt therein is recycled by solid recovery unit 700;Filtrate quilt therein Ice crystal and glacial meltwater are separated into after the recycling sedimentation of ice water tank 800, ice crystal therein is passed through in ripening at low temperature reactor 400 and carries out It cures again, glacial meltwater water quality therein can discharge when reaching effluent quality requirement.It is remaining in equipment for separating liquid from solid 500 Filtrate is passed through in recovery pond 600, and is periodically passed through in ice crystal crystallizer 300 and is recrystallized (second level freezing processing).
Embodiment 1 (curing temperature -15~-20 DEG C, 7 hours curing times)
It is ethyl acetate, NaCl, Na in the ethyl acetate waste liquid main component that pharmaceutical intermediate is synthetically produced2CO3、NaAc And NaOH, ethyl acetate raw water COD are as follows: 77960mg/L.
After level-one freezing processing, concentrate COD is 293000mg/L, and level-one freezing water outlet COD is 10590mg/L. Wherein concentrate accounts for raw water volume 14.0%.
After second level freezing processing, water outlet COD is 2610mg/L for level-one freezing water outlet.
After chilled processing, every liter of waste water energy generates white solid 120g/L, and main ingredient is Na2CO3And NaCl.
Comparative example 1 (curing temperature -15~-20 DEG C, 5 hours curing times)
It is ethyl acetate, NaCl, Na in the ethyl acetate waste liquid main component that pharmaceutical intermediate is synthetically produced2CO3、NaAc And NaOH, ethyl acetate raw water COD are as follows: 77960mg/L.
After level-one freezing processing, concentrate COD is 272500mg/L, and level-one freezing water outlet COD is 11250mg/L. Wherein concentrate accounts for raw water volume 30.5%.
After second level freezing processing, water outlet COD is 2740mg/L for level-one freezing water outlet.
After chilled processing, every liter of waste water energy generates white solid 98g/L, and main ingredient is Na2CO3And NaCl.
Comparative example 2 (curing temperature -15~-20 DEG C, 9 hours curing times)
It is ethyl acetate, NaCl, Na in the ethyl acetate waste liquid main component that pharmaceutical intermediate is synthetically produced2CO3、NaAc And NaOH, ethyl acetate raw water COD are as follows: 77960mg/L.
After level-one freezing processing, concentrate COD is 296500mg/L, and level-one freezing water outlet COD is 10370mg/L. Wherein concentrate accounts for raw water volume 12.0%.
After second level freezing processing, water outlet COD is 2595mg/L for level-one freezing water outlet.
After chilled processing, every liter of waste water energy generates white solid 123g/L, and main ingredient is Na2CO3And NaCl.
Comparative example 3 (curing temperature -10~-15 DEG C, 7 hours curing times)
It is ethyl acetate, NaCl, Na in the ethyl acetate waste liquid main component that pharmaceutical intermediate is synthetically produced2CO3、NaAc And NaOH, ethyl acetate raw water COD are as follows: 77960mg/L.
After level-one freezing processing, concentrate COD is 121200mg/L, and level-one freezing water outlet COD is 12210mg/L. Wherein concentrate accounts for raw water volume 76.0%.
After second level freezing processing, water outlet COD is 2800mg/L for level-one freezing water outlet.
After chilled processing, every liter of waste water energy generates white solid 43g/L, and main ingredient is Na2CO3And NaCl.

Claims (4)

1. a kind of processing system of ethyl acetate waste liquid, which is characterized in that including consisting of part:
Air-floating apparatus, middle tank, the ice crystal crystallizer with slice ice machine, the slaking reaction device, separation of solid and liquid installed in order Device, wherein the liquid separating opening of the equipment for separating liquid from solid is connected with the liquids recovery mouth of a recovery pond, the recovery pond Liquid outlet opening is connected with the ice crystal crystallizer;The solid separating opening of the equipment for separating liquid from solid and a solid recovery unit phase Even;The ice crystal separating opening of the equipment for separating liquid from solid is connected with the ice crystal feed inlet of an ice water tank, and the ice crystal of the ice water tank goes out Material mouth is connected in the ice crystal crystallizer.
2. a kind of processing system of ethyl acetate waste liquid as described in claim 1, which is characterized in that the slaking reaction device For the ripening at low temperature reactor with agitating device.
3. a kind of processing system of ethyl acetate waste liquid as described in claim 1, which is characterized in that the separation of solid and liquid dress It include centrifugal separator in setting.
4. a kind of processing method of ethyl acetate waste liquid as described in any one of working as claim 1-3, which is characterized in that packet Include following steps:
The ethyl acetate waste liquid generated after production, which is pumped into air-floating apparatus, carries out aeration air bearing pretreatment, after being aerated air bearing Waste liquid is discharged into middle tank storage;
Periodically the waste liquid of storage is discharged into ice crystal crystallizer and carries out decrease temperature crystalline, slice ice machine smashes ice crystal, broken Ice crystal is passed through in slaking reaction device and carries out ripening at low temperature 4-8 hours;
Curing separation of the ice crystal through centrifuge in equipment for separating liquid from solid after primary curing, the equipment for separating liquid from solid is by ice crystal In filtrate and salinity separating and recovering, wherein filtrate is discharged into recovery pond, and solid salinity is discharged into solid recovery unit, remaining Ice crystal after centrifugation is discharged into ice water tank;
Filtrate after collecting is recrystallized from being passed through again in ice crystal crystallizer in recovery pond, and the ice crystal after collecting Ripening at low temperature again is carried out after being discharged into slaking reaction device in ice water tank.
CN201910412360.5A 2019-05-17 2019-05-17 A kind of ethyl acetate liquid waste treatment system and its processing method Pending CN110002656A (en)

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CN208362100U (en) * 2018-05-24 2019-01-11 汕头市楷洽化工有限公司 A kind of glycerol production waste liquid recovery apparatus
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