CN110228885A - A kind of sewage-treatment plant for phenol and acetone synthetic reaction - Google Patents
A kind of sewage-treatment plant for phenol and acetone synthetic reaction Download PDFInfo
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- CN110228885A CN110228885A CN201910362407.1A CN201910362407A CN110228885A CN 110228885 A CN110228885 A CN 110228885A CN 201910362407 A CN201910362407 A CN 201910362407A CN 110228885 A CN110228885 A CN 110228885A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/18—Dehydration
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/26—Treatment of water, waste water, or sewage by extraction
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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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
- C02F1/66—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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F2001/007—Processes including a sedimentation step
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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Abstract
The present invention discloses a kind of sewage-treatment plant for phenol and acetone synthetic reaction, by neutralization kettle, oil water separator, subsider, falling film evaporator, rectifying column, the equipment such as evaporative crystallization room are formed by connecting by Tube formation, with low boiling organic matter in the waste water that rectifying column generates, based on sodium sulfate salt, into after falling film evaporator, carry out multiple-effect operation, realize sufficient gas-liquid separation, after high boiling aqueous sodium persulfate solution enters the second evaporative crystallization room, the sodium sulfate crystal generated with the first evaporative crystallization room, it is being centrifugated, after washing, complete the high-purity deduction of sodium sulphate, the rate of recovery is high, it can directly recycle, greatly reduce cost of sewage disposal, phenol removal rate reaches 99.5% or more to sewage after processing, acetone, methanol, the removal rate of CODcr reaches 98.5-99.6%, sodium sulphate Recovery rate reaches 92% or more, and purity is greater than 95%.
Description
Technical field
The present invention relates to chemical wastewater treatment apparatus fields, and in particular to a kind of dirt for phenol and acetone synthetic reaction
Water treatment facilities.
Background technique
Phenol popular name carbolic acid is the crystal that colourless needles or white chunks have fragranced, is production dyestuff, medical intermediate
The important source material of the products such as body, explosive, plastics.Acetone is important organic solvent, while being surfactant again, drug, having
The raw material of machine glass, epoxy resin.Phenol and the common production method of acetone have cumene method, toluol-benzene formic acid method, oxidizing process
Deng.There is 90% or more phenol to produce using cumene method in the world at present, mainly by benzene and propylene alkylation reaction, oxidation,
Four hydrolysis, concentration master operations.
A certain amount of high concentrated organic wastewater can be generated in cumene method production process, main component is phenol, acetone, α-
The poisonous and harmful hardly degraded organic substance such as methylbenzyl alcohol and a large amount of sulfate.Shanghai with 200,000 tons of phenol-acetone annual outputs
Gaoqiao Petrochemical Company, the waste water content in detection device, Contents of Main Components are as follows: phenol 2.6mg/L, formaldehyde 13.7mg/L, methanol
17.2mg/L, acetone 102.9mg/L, isopropylbenzene 6.9mg/L, hydroxyl ketone 343.1mg/L, sodium sulphate 1681.1mg/L.Through grinding
Study carefully discovery, phenol-acetone production waste water mainly there are following characteristics: 1) lacking the nutriments such as N, P, microelement in waste water；2) from
The analysis of the component properties such as phenol, acetone, petroleum-type, these organic matters have biggish solubility in water, such as with physical method
Absorption, stripping etc. are difficult to directly remove；3) salt content is high；4) component all has a degree of biodegradable, but simultaneously
Substrate when reaching a certain concentration, equally have stronger Biostatic, when be more than a certain concentration after will result directly in biology
It is poisoned to death, which has stronger Biostatic, and biology has to pass through stringent domestication, and the strain tamed must have
The characteristic of salt tolerant；5) raw wastewater shows stronger alkalinity, and actual pH has stronger penetrating odor between 9~10.
The phenol-acetone production method for treating wastewater reported both at home and abroad at present has flocculation-absorption-Strong oxdiative method, biological oxidation
Method, room temperature ClO 2 catalyzed oxidation method, electrolysis method combination chemical catalytic oxidation method, catalytic wet oxidation, EFP photoelectronic pulse
Method, the index of COD are≤500mg/L.Existing device and side for the sewage treatment of phenol-acetone synthetic reaction
Method still has following problems: 1, raw material phenol, acetone have good water solubility, almost can with water with arbitrarily than miscible,
More difficult separation；The ingredients such as hydroxy-ketone, formaldehyde, methanol, isopropylbenzene dissolve in organic solvent；Sodium sulphate content is high, separating-purifying
Rate is low, and residual rate is high after processing；2, after the processing of sewage-treatment plant, phenol removal rate is not achieved 99% or more, acetone,
Methanol, CODcr removal rate be not achieved 98% or more；3, the sodium sulphate low yield after crystallization and purification, purity is less than 95%.
Summary of the invention
In order to solve the above technical problems, the purpose of the present invention is to provide one kind to be used for phenol and acetone synthetic reaction
Sewage-treatment plant, by equipment such as neutralization kettle, oil water separator, subsider, falling film evaporator, rectifying column, evaporative crystallization rooms
It is formed by connecting by Tube formation, in the waste water that rectifying column generates based on low boiling organic matter, sodium sulfate salt, into falling film evaporation
After device, multiple-effect operation is carried out, after realizing that sufficient gas-liquid separation, high boiling aqueous sodium persulfate solution enter the second evaporative crystallization room,
The sodium sulfate crystal generated with the first evaporative crystallization room is completed the high-purity deduction of sodium sulphate, is returned after centrifuge separation, washing
High income can be recycled directly, greatly reduce cost of sewage disposal, phenol removal rate reaches sewage after processing
99.5% or more, acetone, methanol, CODcr removal rate reach 98.5-99.6%, sodium sulphate recovery rate reaches 92% or more, pure
Degree is greater than 95%.
The purpose of the present invention can be achieved through the following technical solutions:
The present invention provides a kind of sewage-treatment plant for phenol and acetone synthetic reaction, including first neutralize kettle,
First water circular chamber, oil water separator, circulation alkali liquor tower, rectifying column, second neutralize kettle, falling film evaporator, and described first neutralizes
NaOH solution is filled in kettle, the sewage for will generate during cumene method synthesizing phenol acetone carries out neutralization reaction；First
The bottom for neutralizing kettle is connect with the first water circular chamber by pipeline, and the side wall of the first neutralization kettle is connected with liquid relief pump by pipeline,
First water circular chamber and oil water separator are pumped by liquid relief to be connected；
The first water circular chamber, which is used to neutralize the solid phase precipitation object that kettle generates for first, carries out the stirring of water circulating-heating；Institute
It states liquid relief pump and distills condensed liquid phase part sucking oil water separator for neutralizing kettle for first；
The first water circular chamber is connected with the first evaporative crystallization room by pipeline, and oil water separator is connected with by pipeline
Tar recycling can and subsider；The tar that tar recycling can is used to generate oil water separator is recycled, and subsider is used
Counter-current extraction removing phenol is carried out in the water layer generated to oil water separator；
The subsider is connected with circulation alkali liquor tower by pipeline, and circulation alkali liquor tower is connected with lye by pipeline and settles
Slot, second neutralize kettle, and lye subsider is connected with rectifying column by pipeline；
The circulation alkali liquor tower is used to carry out alkali cleaning to the water layer after removing phenol；The rectifying column is used to settle lye
The water phase that slot back extraction generates carries out rectifying；Described second, which neutralizes kettle, is used to carry out neutralization reaction to circulation alkali liquor；
The rectifying column is connected with falling film evaporator, the second evaporative crystallization room, centrifuge separation room, washing in turn by pipeline
Room.
As a further solution of the present invention, the rectifying column is connected with acetone recycling can, Methanol Recovery tank by pipeline.
As a further solution of the present invention, first evaporative crystallization room is connect by pipeline with centrifuge separation room, the
The crystal that one evaporative crystallization room and the second evaporative crystallization room generate obtains solid after being centrifuged the separating, washing of room, washing chamber
Sodium sulfate crystal.
As a further solution of the present invention, in the sewage generated during the cumene method synthesizing phenol acetone, respectively
The content of main component is as follows: acetone 80-110mg/L, hydroxy-ketone 320-360mg/L, phenol 6-15mg/L, formaldehyde 15-18mg/
L, methanol 16-20mg/L, isopropylbenzene 5-10mg/L, sodium sulphate 3200-3800mg/L.
As a further solution of the present invention, the falling film evaporator include outer barrel, upper perforated plate, lower perforated plate, inner cylinder,
Falling film evaporation channel, the outer wall top of outer barrel are equipped with material inlet, and heating steam inlet is equipped in the middle part of outer wall, is set on the downside of outer wall
There is condensation-water drain；
The section in the falling film evaporation channel has upper steady section, lower steady section, curved sections, and curved sections are symmetricly set on this
The two sides of falling film evaporator central axes, upper steady section are set to the top of curved sections, and lower steady section is set to the bottom of curved sections.
As a further solution of the present invention, the curved sections are in several continuous arc shapeds, and the arc from centre to two sides
The radian of line constantly reduces with arc length.
As a further solution of the present invention, the heat being equipped in the outer barrel around the setting of falling film evaporation channels peripheral is steamed
The one end in steam pipe road, vapours pipeline is connect with heating steam inlet.
As a further solution of the present invention, the working method of the sewage-treatment plant is as follows:
S1, the sewage that will be generated during cumene method synthesizing phenol acetone, are passed through fill the first of NaOH solution together
It neutralizes kettle and carries out neutralization reaction, distill 40-50min at 100-105 DEG C, so that the solid phase precipitation object that generates of neutralization reaction is from bottom
It is passed through the first water circular chamber after releasing, distills condensed liquid phase part and uses liquid relief pump sucking oil water separator；
S2, the first water is recycled to indoor circulating water heating to 80-90 DEG C, after mechanical stirring 30-40min, stratification,
Water layer is passed through the first evaporative crystallization room, and oil reservoir is passed through oil water separator；
S3, oil water separator carry out continuous water-oil separating, and oil reservoir is the tar containing phenol type organic, are conveyed into coke
Oil recovery tank is recycled；Water layer is passed through subsider and carries out counter-current extraction removing phenol；
Water layer after S4, removing phenol is passed through circulation alkali liquor tower and carries out alkali cleaning, and lye subsider is passed through after alkali cleaning and is carried out instead
Extraction, be stripped generation water phase be sent into rectifying column, circulation alkali liquor be passed through fill hydrochloric acid solution second neutralization kettle neutralized
Reaction；
S5, rectifying column rectifying extract the low boilings organic components such as acetone, methanol；
S6, rectifying column waste water from tower reactor flow out, be sent into falling film evaporator, removing low boiling is evaporated at 85-95 DEG C
Organic matter is re-fed into the second evaporative crystallization room and crystallizes, and crystal is centrifuged with the crystal generated with the first evaporative crystallization room
Room, washing chamber separating, washing after obtain solid sulphuric acid sodium crystal.
Beneficial effects of the present invention:
1, the sewage-treatment plant for phenol and acetone synthetic reaction of the invention by neutralization kettle, oil water separator, sinks
The equipment such as drop slot, falling film evaporator, rectifying column, evaporative crystallization room are formed by connecting by Tube formation, the waste water that rectifying column generates
In based on low boiling organic matter, sodium sulfate salt, into after falling film evaporator, carry out multiple-effect operation, realize sufficient gas-liquid separation,
High boiling aqueous sodium persulfate solution enter the second evaporative crystallization room after, with the first evaporative crystallization room generate sodium sulfate crystal, from
After heart separation, washing, the high-purity deduction of sodium sulphate is completed, the rate of recovery is high, can directly recycle, greatly reduce sewage
Processing cost, phenol removal rate reaches 99.5% or more to sewage after processing, acetone, methanol, CODcr removal rate reach
98.5-99.6%, sodium sulphate recovery rate reach 92% or more, and purity is greater than 95%.
2, sewage is passed through the first neutralization kettle for filling NaOH solution, and remaining sulfuric acid can be reacted with sodium hydroxide generates sulfuric acid
Sodium salt, so that the ingredients such as a large amount of low boiling acetone, methanol, methanol, water become steam, condensation is formed the distillation at 100-105 DEG C
Sucking oil water separator is pumped by liquid relief after liquid phase；Can there are a large amount of sodium sulphate and high boiling organic components in solid phase precipitation object,
Convenient separation and purification to sodium sulphate in solid phase precipitation object.
3, after solid phase precipitation object enters the first water circular chamber, cooperative mechanical stirring, enough water can be by oversaturated sulphur
Sour sodium dissolves, and after stratification, the oil reservoir that sodium sulphate unsaturated solution can be formed with organic matters such as phenol, hydroxy-ketones is layered, oil
Soluble substance also can be well into oil reservoir, and the water layer into evaporative crystallization room can evaporate moisture, so that high concentration, high-purity
Sulfate crystal polymerization, remove moisture.
4, after the oil reservoir containing phenol, hydroxy-ketone enters oil water separator, the water-oil separating that can be further refined,
Most phenol can enter oil reservoir, can be recycled after collection；There are still small contents, good water solubility in water layer
Phenol can remove phenol by counter-current extraction.
5, in falling film evaporator, heating steam improves the convective heat transfer effect of heating steam by way of around heating
Rate reduces the sinuous flow and dosage cost of steam, improves the evaporation and concentration efficiency of falling film evaporator.
Detailed description of the invention
The present invention will be further described below with reference to the drawings.
Fig. 1 is structural schematic diagram of the present invention for phenol and the sewage-treatment plant of acetone synthetic reaction, wherein arrow
Indicate the flow direction of ingredient in sewage.
Fig. 2 is the cross section view of falling film evaporator of the present invention.
In figure: 1, first neutralizing kettle；2, the first water circular chamber；3, liquid relief pumps；4, oil water separator；5, the first evaporative crystallization
Room；6, tar recycling can；7, subsider；8, circulation alkali liquor tower；9, lye subsider；10, rectifying column；11, second kettle is neutralized；
12, acetone recycling can；13, Methanol Recovery tank；14, falling film evaporator；15, the second evaporative crystallization room；16, it is centrifugated room；17,
Washing chamber；141, outer barrel；142, upper perforated plate；143, lower perforated plate；144, inner cylinder；145, falling film evaporation channel；146, raw material
Import；147, steam inlet is heated；148, condensation-water drain；149, upper steady section；150, lower steady section；151, curved sections；
152, vapours pipeline.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts all other
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1
Refering to fig. 1 shown in -2, the present embodiment provides a kind of sewage-treatment plant for phenol and acetone synthetic reaction, packets
It includes the first neutralization kettle 1, the first water circular chamber 2, oil water separator 4, circulation alkali liquor tower 8, rectifying column 10, second and neutralizes kettle 11, drop
Film evaporator 14.
Wherein, NaOH solution is filled in the first neutralization kettle 1, for generate cumene method synthesizing phenol acetone in the process
Sewage carries out neutralization reaction；The bottom of first neutralization kettle 1 is connect with the first water circular chamber 2 by pipeline, and first neutralizes the side of kettle 1
Wall is connected with liquid relief pump 3 by pipeline, and the first water circular chamber 2 is connect with oil water separator 4 by liquid relief pump 3.First water circulation
Room 2 is used to the solid phase precipitation object that the first neutralization kettle 1 generates carrying out the stirring of water circulating-heating；The liquid relief pump 3 is used for first
It neutralizes kettle 1 and distills condensed liquid phase part sucking oil water separator 4.
First water circular chamber 2 is connected with the first evaporative crystallization room 5 by pipeline, and oil water separator 4 is connected with by pipeline
Tar recycling can 6 and subsider 7；The tar that tar recycling can 6 is used to generate oil water separator 4 is recycled, and is settled
The water layer that slot 7 is used to generate oil water separator 4 carries out counter-current extraction removing phenol.Subsider 7 is connected with circulation by pipeline
Washing tower 8, circulation alkali liquor tower 8 are connected with lye subsider 9, second by pipeline and neutralize kettle 11, and lye subsider 9 passes through pipeline
It is connected with rectifying column 10.
Circulation alkali liquor tower 8 is used to carry out alkali cleaning to the water layer after removing phenol；The rectifying column 10 is used to settle lye
The water phase that the back extraction of slot 9 generates carries out rectifying；Described second, which neutralizes kettle 11, is used to carry out neutralization reaction to circulation alkali liquor.
Rectifying column 10 by pipeline be connected in turn falling film evaporator 14, the second evaporative crystallization room 15, centrifuge separation room 16,
Washing chamber 17, first evaporative crystallization room 5 are connect by pipeline with centrifuge separation room 16, the first evaporative crystallization room 5 and second
The crystal that evaporative crystallization room 15 generates obtains solid sulphuric acid sodium crystal after being centrifuged the separating, washing of room 16, washing chamber 17.
As shown in fig.2, falling film evaporator 14 include outer barrel 141, upper perforated plate 142, lower perforated plate 143, inner cylinder 144,
Falling film evaporation channel 145, the outer wall top of outer barrel 141 are equipped with material inlet 146, heating steam inlet are equipped in the middle part of outer wall
147, outer wall downside is equipped with condensation-water drain 148.The section in falling film evaporation channel 145 has upper steady section 149, lower steady section
150, curved sections 151, curved sections 151 are symmetricly set on the two sides of the falling film evaporator central axes, and upper steady section 149 is set to curved surface
The top of section 151, lower steady section 150 are set to the bottom of curved sections 151.Curved sections 151 are in several continuous arc shapeds, and from centre
Radian to the camber line of two sides constantly reduces with arc length.It is equipped in outer barrel 141 around the 145 periphery setting of falling film evaporation channel
One end of vapours pipeline 152, vapours pipeline 152 is connect with heating steam inlet 147.
Tower bottom of rectifying tower outflow waste water entered in outer barrel 141 from material inlet 146, heating steam from heating steam into
Mouth 147 enters in inner cylinder 144, will be from upper perforated plate 142 when the liquid level of feed liquid in inner cylinder 144 increases at upper perforated plate 142
It flows into falling film evaporation channel 145,145 inner wall of falling film evaporation channel will form non-uniform ring-shaped liquid film, and ring-shaped liquid film is in weight
It can be formed by helical duct along the inner wall of curved sections 151 when flowing downward under power effect, periodically change speed and direction,
With the variation tendency of cambered surface, evaporation solution is made to be in the sinuous flow state for first increasing, reducing afterwards always.In helical falling-film evaporator
In, ring-shaped liquid film absorbs rapidly the thermal energy of steam in vapours pipeline 152 during flowing downward, and makes liquid film temperature liter
Height reaches boiling point evaporation, and the secondary steam for evaporating generation is detached from the center for entering falling film evaporation channel 145 from liquid film surface, and
Drive 151 inner wall ring-shaped liquid film of curved sections helical flow downwardly together.In helical falling-film evaporator, heating steam is by surrounding
The mode of heating improves the convective heat transfer efficiency of heating steam, reduces the sinuous flow and dosage cost of steam, improve falling liquid film
Evaporator is concentrated by evaporation efficiency.
Embodiment 2
Refering to fig. 1 shown in -2, the present embodiment provides a kind of sewage treatment sides suitable for phenol and acetone synthetic reaction
Method, specifically includes the following steps:
S1, the sewage that will be generated during cumene method synthesizing phenol acetone, are passed through fill the first of NaOH solution together
It neutralizes kettle 1 and carries out neutralization reaction, distill 40-50min at 100-105 DEG C, so that the solid phase precipitation object that generates of neutralization reaction is from kettle
Bottom is passed through the first water circular chamber 2 after releasing, and distills condensed liquid phase part and uses 3 sucking oil water separator 4 of liquid relief pump；Its
In, the content of each main component is as follows in sewage: acetone 80-110mg/L, hydroxy-ketone 320-360mg/L, phenol 6-15mg/L,
Formaldehyde 15-18mg/L, methanol 16-20mg/L, isopropylbenzene 5-10mg/L, sodium sulphate 3200-3800mg/L；
The sewage generated during cumene method synthesizing phenol acetone, by composition detection, the main component contained is third
Ketone, hydroxy-ketone, phenol, formaldehyde, methanol, isopropylbenzene, sodium sulphate, and the content of acetone, hydroxy-ketone, sodium sulphate is very high, separation
Difficulty is big；Raw material phenol, acetone have good water solubility, almost can be with water arbitrarily than miscible, it is more difficult to separate；Hydroxyl
The ingredients such as ketone, formaldehyde, methanol, isopropylbenzene dissolve in organic solvent；Sodium sulphate content is high, and separating-purifying rate is low, residual after processing
Stay rate height.For step S1 of the present invention in view of using strong acid sulfuric acid catalysis in hydrolysis, the pH value of sewage is first passed through Sheng in acidity
Have NaOH solution first neutralizes kettle, and remaining sulfuric acid can be reacted with sodium hydroxide generates sodium sulfate salt, the steaming at 100-105 DEG C
It evaporates so that the ingredients such as a large amount of low boiling acetone, methanol, methanol, water become steam, condensation forms after liquid phase and pumps sucking oil by liquid relief
Separator；Can there are a large amount of sodium sulphate and high boiling organic components in solid phase precipitation object, it is convenient to sulphur in solid phase precipitation object
The separation and purification of sour sodium.
S2, by the circulating water heating in the first water circular chamber 2 to 80-90 DEG C, after mechanical stirring 30-40min, stand point
Layer, water layer are passed through the first evaporative crystallization room 5, and oil reservoir is passed through oil water separator 4；
After solid phase precipitation object enters the first water circular chamber, cooperative mechanical stirring, enough water can be by oversaturated sulphur
Sour sodium dissolves, and after stratification, the oil reservoir that sodium sulphate unsaturated solution can be formed with organic matters such as phenol, hydroxy-ketones is layered, oil
Soluble substance also can be well into oil reservoir, and the water layer into evaporative crystallization room can evaporate moisture, so that high concentration, high-purity
Sulfate crystal polymerization, remove moisture.
S3, oil water separator 4 carry out continuous water-oil separating, and oil reservoir is the tar containing phenol type organic, are conveyed into
Tar recycling can 6 is recycled；Water layer is passed through subsider 7 and carries out counter-current extraction removing phenol；
After the oil reservoir containing phenol, hydroxy-ketone enters oil water separator, the water-oil separating that can be further refined,
Most phenol can enter oil reservoir, can be recycled after collection；There are still small contents, good water solubility in water layer
Phenol can remove phenol by counter-current extraction.
Water layer after S4, removing phenol is passed through circulation alkali liquor tower 8 and carries out alkali cleaning, and the progress of lye subsider 9 is passed through after alkali cleaning
Back extraction, be stripped generation water phase be sent into rectifying column 10, circulation alkali liquor be passed through fill hydrochloric acid solution second neutralize kettle 11 into
Row neutralization reaction；
Fraction sodium sulphate is still had in water layer, the ingredients such as a large amount of acetone, methanol, further alkali cleaning can be by water layer
In residual phenylol originally remove completely, into after rectifying column, the separating-purifying of acetone, methanol can be carried out.
S5,10 rectifying of rectifying column extract the low boilings organic components such as acetone, methanol, be respectively fed to acetone recycling can 12,
Methanol Recovery tank 13 is recycled；
S6, rectifying column 10 waste water from tower reactor flow out, be sent into falling film evaporator 14, removing is evaporated at 85-95 DEG C
Low boiling organic matter, is re-fed into the inner crystallization in the second evaporative crystallization room 15, crystal and the crystal generated with the first evaporative crystallization room 5 pass through from
Heart separation chamber 16, washing chamber 17 separating, washing after obtain solid sulphuric acid sodium crystal.
In the waste water that rectifying column generates based on low boiling organic matter, sodium sulfate salt, into after falling film evaporator, multiple-effect is carried out
Operation, after realizing that sufficient gas-liquid separation, high boiling aqueous sodium persulfate solution enter the second evaporative crystallization room, with the first evaporative crystallization
The sodium sulfate crystal that room generates completes the high-purity deduction of sodium sulphate, the rate of recovery is high, can be direct after centrifuge separation, washing
It recycles, greatly reduces cost of sewage disposal.
In the description of this specification, the description of reference term " one embodiment ", " example ", " specific example " etc. means
Particular features, structures, materials, or characteristics described in conjunction with this embodiment or example are contained at least one implementation of the invention
In example or example.In the present specification, schematic expression of the above terms may not refer to the same embodiment or example.
Moreover, particular features, structures, materials, or characteristics described can be in any one or more of the embodiments or examples to close
Suitable mode combines.
Above content is only citing made for the present invention and explanation, affiliated those skilled in the art are to being retouched
The specific embodiment stated does various modifications or additions or is substituted in a similar manner, and without departing from invention or surpasses
More range defined in the claims, is within the scope of protection of the invention.
Claims (8)
1. a kind of sewage-treatment plant for phenol and acetone synthetic reaction, including the first neutralization kettle (1), the first water circular chamber
(2), oil water separator (4), circulation alkali liquor tower (8), rectifying column (10), second neutralize kettle (11), falling film evaporator (14), special
Sign is, NaOH solution is filled in first neutralization kettle (1), for generate cumene method synthesizing phenol acetone in the process
Sewage carries out neutralization reaction；First bottom for neutralizing kettle (1) is connect with the first water circular chamber (2) by pipeline, and first neutralizes kettle
(1) side wall is connected with liquid relief pump (3) by pipeline, and the first water circular chamber (2) and oil water separator (4) pass through liquid relief pump (3)
Connection；
The first water circular chamber (2), which is used to neutralize the solid phase precipitation object that kettle (1) generates for first, carries out the stirring of water circulating-heating；
The liquid relief pump (3), which is used to neutralize kettle (1) for first, distills condensed liquid phase part sucking oil water separator (4)；
The first water circular chamber (2) is connected with the first evaporative crystallization room (5) by pipeline, and oil water separator (4) passes through pipeline
It is connected with tar recycling can (6) and subsider (7)；The tar that tar recycling can (6) is used to generate oil water separator (4) is subject to
It recycles, the water layer that subsider (7) is used to generate oil water separator (4) carries out counter-current extraction removing phenol；
The subsider (7) is connected with circulation alkali liquor tower (8) by pipeline, and circulation alkali liquor tower (8) is connected with lye by pipeline
Subsider (9), second neutralize kettle (11), and lye subsider (9) is connected with rectifying column (10) by pipeline；
The circulation alkali liquor tower (8) is used to carry out alkali cleaning to the water layer after removing phenol；The rectifying column (10) is used for lye
The water phase that subsider (9) back extraction generates carries out rectifying；Described second, which neutralizes kettle (11), is used to carry out circulation alkali liquor to neutralize instead
It answers；
The rectifying column (10) is connected with falling film evaporator (14), the second evaporative crystallization room (15), centrifugation point in turn by pipeline
From room (16), washing chamber (17).
2. the sewage-treatment plant according to claim 1 for phenol and acetone synthetic reaction, which is characterized in that described
Rectifying column (10) is connected with acetone recycling can (12), Methanol Recovery tank (13) by pipeline.
3. the sewage-treatment plant according to claim 1 for phenol and acetone synthetic reaction, which is characterized in that described
First evaporative crystallization room (5) is connect by pipeline with centrifuge separation room (16), the first evaporative crystallization room (5) and the second evaporative crystallization
The crystal that room (15) generates obtains solid sulphuric acid sodium crystal after being centrifuged the separating, washing of room (16), washing chamber (17).
4. the sewage-treatment plant according to claim 1 for phenol and acetone synthetic reaction, which is characterized in that described
In the sewage generated during cumene method synthesizing phenol acetone, the content of each main component is as follows: acetone 80-110mg/L, hydroxyl
Base ketone 320-360mg/L, phenol 6-15mg/L, formaldehyde 15-18mg/L, methanol 16-20mg/L, isopropylbenzene 5-10mg/L, sulfuric acid
Sodium 3200-3800mg/L.
5. the sewage-treatment plant according to claim 1 for phenol and acetone synthetic reaction, which is characterized in that described
Falling film evaporator (14) includes that outer barrel (141), upper perforated plate (142), lower perforated plate (143), inner cylinder (144), falling film evaporation are logical
The outer wall top in road (145), outer barrel (141) is equipped with material inlet (146), and heating steam inlet (147) is equipped in the middle part of outer wall,
Condensation-water drain (148) are equipped on the downside of outer wall；
The section of the falling film evaporation channel (145) has upper steady section (149), lower steady section (150), curved sections (151), bent
Face section (151) is symmetricly set on the two sides of the falling film evaporator central axes, and upper steady section (149) is set to the top of curved sections (151)
Portion, lower steady section (150) are set to the bottom of curved sections (151).
6. the sewage-treatment plant according to claim 5 for phenol and acetone synthetic reaction, which is characterized in that described
Curved sections (151) are in several continuous arc shapeds, and the radian of the camber line from centre to two sides constantly reduces with arc length.
7. the sewage-treatment plant according to claim 5 for phenol and acetone synthetic reaction, which is characterized in that described
The vapours pipeline (152) around the setting of falling film evaporation channel (145) periphery, vapours pipeline are equipped in outer barrel (141)
(152) one end is connect with heating steam inlet (147).
8. the sewage-treatment plant according to claim 1 for phenol and acetone synthetic reaction, which is characterized in that the dirt
The working method of water treatment facilities is as follows:
S1, the sewage for generating cumene method synthesizing phenol acetone in the process are passed through the first neutralization for filling NaOH solution together
Kettle (1) carries out neutralization reaction, distills 40-50min at 100-105 DEG C, so that the solid phase precipitation object that generates of neutralization reaction is from bottom
It is passed through the first water circular chamber (2) after releasing, distills condensed liquid phase part and uses liquid relief pump (3) sucking oil water separator (4)；
S2, by the circulating water heating in the first water circular chamber (2) to 80-90 DEG C, after mechanical stirring 30-40min, stratification,
Water layer is passed through the first evaporative crystallization room (5), and oil reservoir is passed through oil water separator (4)；
S3, oil water separator (4) carry out continuous water-oil separating, and oil reservoir is the tar containing phenol type organic, are conveyed into coke
Oil recovery tank (6) is recycled；Water layer is passed through subsider (7) and carries out counter-current extraction removing phenol；
Water layer after S4, removing phenol is passed through circulation alkali liquor tower (8) and carries out alkali cleaning, and lye subsider (9) progress is passed through after alkali cleaning
Back extraction, the water phase for being stripped generation are sent into rectifying column (10), and circulation alkali liquor is passed through the second neutralization kettle for filling hydrochloric acid solution
(11) neutralization reaction is carried out；
S5, rectifying column (10) rectifying extract the low boilings organic components such as acetone, methanol；
S6, rectifying column (10) waste water from tower reactor flow out, be sent into falling film evaporator (14), removing is evaporated at 85-95 DEG C
Low boiling organic matter, is re-fed into that the second evaporative crystallization room (15) is inner to be crystallized, crystal and the crystal generated with the first evaporative crystallization room (5)
Solid sulphuric acid sodium crystal is obtained after being centrifuged the separating, washing of room (16), washing chamber (17).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112209467A (en) * | 2020-09-23 | 2021-01-12 | 吉化集团油脂化工有限公司 | Phenol-containing wastewater treatment method of phenol-acetone device |
| CN112707460A (en) * | 2020-12-29 | 2021-04-27 | 国网河北省电力有限公司电力科学研究院 | Vertical falling film equipment for sewage desulfurization of thermal power plant |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104190697A (en) * | 2014-09-19 | 2014-12-10 | 山东腾跃化学危险废物研究处理有限公司 | Resourceful treatment method for hazardous wastes containing water soluble salts and organic matters |
| CN104876379A (en) * | 2015-05-07 | 2015-09-02 | 中石化上海工程有限公司 | Method for treating wastewater by dicumyl peroxide DCP device |
| CN107823903A (en) * | 2017-12-07 | 2018-03-23 | 江苏迈克化工机械有限公司 | A kind of helical falling-film evaporator |
-
2019
- 2019-04-30 CN CN201910362407.1A patent/CN110228885A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104190697A (en) * | 2014-09-19 | 2014-12-10 | 山东腾跃化学危险废物研究处理有限公司 | Resourceful treatment method for hazardous wastes containing water soluble salts and organic matters |
| CN104876379A (en) * | 2015-05-07 | 2015-09-02 | 中石化上海工程有限公司 | Method for treating wastewater by dicumyl peroxide DCP device |
| CN107823903A (en) * | 2017-12-07 | 2018-03-23 | 江苏迈克化工机械有限公司 | A kind of helical falling-film evaporator |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112209467A (en) * | 2020-09-23 | 2021-01-12 | 吉化集团油脂化工有限公司 | Phenol-containing wastewater treatment method of phenol-acetone device |
| CN112707460A (en) * | 2020-12-29 | 2021-04-27 | 国网河北省电力有限公司电力科学研究院 | Vertical falling film equipment for sewage desulfurization of thermal power plant |
| CN112707460B (en) * | 2020-12-29 | 2022-07-15 | 国网河北省电力有限公司电力科学研究院 | Vertical falling film equipment for sewage desulfurization of thermal power plant |
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