CN109879471A - In a kind of n-butyl acrylate and COD treatment process drops in waste water drop COD processing unit and waste water - Google Patents
In a kind of n-butyl acrylate and COD treatment process drops in waste water drop COD processing unit and waste water Download PDFInfo
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- CN109879471A CN109879471A CN201910026127.3A CN201910026127A CN109879471A CN 109879471 A CN109879471 A CN 109879471A CN 201910026127 A CN201910026127 A CN 201910026127A CN 109879471 A CN109879471 A CN 109879471A
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Abstract
The invention discloses in a kind of n-butyl acrylate and waste water drop COD processing unit and waste water drop COD treatment process, processing unit includes butyl acrylate reaction kettle, water surge tank, phase-splitter, polymerization inhibitor tank, crude acrylic acid N-butyl tank, acid solution tank, forced circulation pump, cyclically charging pump, water surge tank is connected to by mixer with the first feed pipe of phase-splitter, butyl acrylate reaction kettle, polymerization inhibitor tank, crude acrylic acid N-butyl tank is connected to the second feed pipe simultaneously, acid solution tank is connected to the input terminal pipeline of mixer, the input terminal of forced circulation pump is connected to phase-splitter pipeline with output end；The oil of phase-splitter is mutually connected to the input terminal pipeline of charge pump is forced, and the output end of charge pump is forced to be connected to the second feed pipe；Treatment process includes neutralizing acidification, purification by liquid extraction and stratification.Dropping COD processing unit and waste water drop COD treatment process with waste water in n-butyl acrylate of the invention has the characteristics that raw material consumption is low, COD reducing effect is good and process modification is simple.
Description
Technical field
The present invention relates to waste water to drop COD treatment process technical field, drops in especially a kind of n-butyl acrylate with waste water
COD treatment process drops in COD processing unit and waste water.
Background technique
N-butyl acrylate is as a kind of important industrial chemicals, a kind of extensive polymeric precursor of use.China at present
Have become the maximum country of production capacity of butyl acrylate.The mature production technology of butyl acrylate is stablized, and what is mainly taken is
Acrylic acid and the butanol esterification under acid catalysis obtain, and mainstream catalyst is p-methyl benzenesulfonic acid, methane sulfonic acid etc. at present, take
In the Catalytic processes, extraction and recovery is carried out to catalyst and is neutralized to wash, under alkaline condition, make acrylic acid in waste water at
Salt, and increase the solubility of alcohol in water, so that largely discharging the higher waste water of COD content in technical process, COD is about 4
×104-6×104Mg/L, on the one hand high COD increases post processing cost, and on the other hand high COD increases material loss.
Fig. 1 is traditional handicraft schematic device, and the neutralization waste water after butyl acrylate neutralization only passes through Sewage treatment tower will
The a small amount of organic matters (such as butanol, butyl ester) contained in waste water are distilled to recover, without acidification, at (such as propylene of salt
Acid sodium-salt, sodium alkoxide etc.) it cannot not recycle.
Summary of the invention
It is of the invention it is main be designed to provide in a kind of n-butyl acrylate and waste water drop COD processing unit and its
COD treatment process drops in waste water, has the characteristics that raw material consumption is low, COD reducing effect is good and process modification is simple.
The present invention can be achieved through the following technical solutions:
The invention discloses drop COD processing unit, including butyl acrylate reaction kettle, water with waste water in a kind of n-butyl acrylate
Surge tank, phase-splitter, polymerization inhibitor tank, crude acrylic acid N-butyl tank, acid solution tank, forced circulation pump, cyclically charging pump, the water
Surge tank is connected to by mixer with the first feed pipe of the phase-splitter, the butyl acrylate reaction kettle, polymerization inhibitor tank,
Crude acrylic acid N-butyl tank is connected to the second feed pipe simultaneously, and the acid solution tank is connected to the input terminal pipeline of mixer,
The input terminal of the forced circulation pump is connected to the phase-splitter pipeline with output end；The oil of the phase-splitter mutually with it is described strong
The input terminal pipeline of charge pump processed is connected to, and the output end for forcing charge pump is connected to second feed pipe.
Further, the waste water output channel company of the input terminal of the water surge tank and neutralizing tower, dehydrating tower, lightness-removing column
It is logical, the neutralizing tower, dehydrating tower, lightness-removing column pH value of waste water be 8.0~11.0.
Further, the first control valve, the acid are equipped between the butyl acrylate reaction kettle and the second feed pipe
It is equipped with the second control valve between NaOH solution tank NaOH and the mixer, pH sensor, first control are equipped with inside the phase-splitter
Valve, the second control valve are connect with the pH sensor simultaneously.
Further, the water phase output end of the phase-splitter is connected to Sewage treatment tower tube road.
Further, the phase-splitter is the phase-splitter with partition.
Another aspect of the present invention is the waste water drop COD treatment process disclosed using above-mentioned wastewater treatment equipment,
The following steps are included:
(1) it neutralizes acidification: alkaline water technique waste water is mixed to neutralization acidification with acid solution；
2) purification by liquid extraction: crude acrylic acid N-butyl is added in the mixture for neutralizing acidification, and purification by liquid extraction is carried out in phase-splitter；
3) stratification: standing separates oily phase and water phase, and oil is mutually recycled and is returned reaction kettle, and water phase is sent to waste water and returns
Tower is received further to recycle.
The present invention drops COD technique and device for increase in the wastewater treatment in current n-butyl acrylate production technology,
Will be more advantageous to material consumption and wastewater treatment than prior art, neutralization waste water COD, which is finally discharged maximum and can reduce, surpasses 60%.
Further, step (1) neutralize acidification in, neutralization be adjusted to pH be 6~7, acid solution be sulphur, carbonic acid, nitric acid and/
Or hydrochloric acid, acid solution molar concentration >=1mol/L.
Further, in step (2) purification by liquid extraction, crude acrylic acid N-butyl is as extractant, extractant additional amount and mixed
The mass ratio for closing waste water is 1:3~1:10, and crude acrylic acid N-butyl is that the content that device generates is more than 95% crude product, and extracts
It takes containing polymerization inhibitor in agent, the extraction residence time is 2~10min.
Further, in step (3) stratification, oil phasor is stablized when keeping standing split-phase, and makes the grease in standing
Split-phase mass ratio is 1:3~1:10.
Further, the polymerization inhibitor be ZJ-701, it is phenthazine, p methoxy phenol, one or two kinds of in hydroquinone
Above mixture；The addition dosage of the polymerization inhibitor are as follows: content in extract liquor is made to maintain 0.02~0.04wt%.
In the present invention, phase-splitter has partition, and mixed liquor is made to carry out multiple split-phase, and the rightmost side of phase-splitter has been the
Split-phase three times, it is nonetheless possible to have it is few can water phase can branch away, therefore in last phase separation chamber, bottom be provided with can lead to it is useless
Water spare interface (, it is daily be it is normally closed, only occur bleeding off again when apparent water phase), connect at higher position it is oily mutually export,
In phase-splitter, oily phase density is low, on upper layer.
In n-butyl acrylate of the present invention and waste water drop COD processing unit and waste water drop COD treatment process have have as follows
The technical effect of benefit:
COD treatment process is dropped using wastewater treatment equipment of the invention and waste water, has recycled the ionized raw material of original process, from
And raw material consumption is reduced, the amount that COD content reduces is exactly that the amount of consumption of raw materials reduction is saved per hour in terms of 100,000 tons of devices
40-200kg raw material, and declined using the waste water COD content being ultimately sent in cesspool (by 4 × 104~6 × 104Mg/L is reduced
To 2 × 104~3 × 104Mg/L).
On technique is realisation, it is molten that the device of the invention need to only increase acid on the basis of science and engineering process and equipment (Fig. 1) of original place
Flow container realizes that neutralizing acidification can be realized, and have stronger realizability, and the effect highly significant of acquirement has more excellent
Promotional value, effective protection environment.
Detailed description of the invention
Attached drawing 1 is traditional handicraft schematic device；
Attached drawing 2 is that the schematic diagram that COD processing unit drops in COD drops in the waste water that neutralizes increased in the present invention in traditional handicraft；
Attached drawing 3 is in a kind of n-butyl acrylate of the present invention and the schematic diagram of COD processing unit drops in waste water.
Specific embodiment
In order that those skilled in the art will better understand the technical solution of the present invention, below with reference to embodiment and to this
Invention product is described in further detail.
As shown in Figure 2 and Figure 3, the invention discloses in a kind of n-butyl acrylate and waste water drop COD processing unit, including
Butyl acrylate reaction kettle, water surge tank, phase-splitter, polymerization inhibitor tank, crude acrylic acid N-butyl tank, acid solution tank, forced circulation
Pump, cyclically charging pump, the water surge tank are connected to by mixer with the first feed pipe of the phase-splitter, the acrylic acid
Butyl ester reaction kettle, polymerization inhibitor tank, crude acrylic acid N-butyl tank are connected to the second feed pipe simultaneously, the acid solution tank with mix
The input terminal pipeline of device is connected to, and the input terminal of the forced circulation pump is connected to the phase-splitter pipeline with output end；It is described
The oil of phase-splitter is mutually connected to the input terminal pipeline for forcing charge pump, the output end and described second for forcing charge pump
Feed pipe connection.
Further, the waste water output channel company of the input terminal of the water surge tank and neutralizing tower, dehydrating tower, lightness-removing column
It is logical, the neutralizing tower, dehydrating tower, lightness-removing column pH value of waste water be 8.0~11.0.
Further, the first control valve, the acid are equipped between the butyl acrylate reaction kettle and the second feed pipe
It is equipped with the second control valve between NaOH solution tank NaOH and the mixer, pH sensor, first control are equipped with inside the phase-splitter
Valve, the second control valve are connect with the pH sensor simultaneously.
Further, the water phase output end of the phase-splitter is connected to Sewage treatment tower tube road.
Further, the phase-splitter is the phase-splitter with partition.
Another aspect of the present invention is the waste water drop COD treatment process disclosed using above-mentioned wastewater treatment equipment,
The following steps are included:
(1) it neutralizes acidification: alkaline water technique waste water is mixed to neutralization acidification with acid solution；
2) purification by liquid extraction: crude acrylic acid N-butyl is added in the mixture for neutralizing acidification, and purification by liquid extraction is carried out in phase-splitter；
3) stratification: standing separates oily phase and water phase, and oil is mutually recycled and is returned reaction kettle, and water phase is sent to waste water and returns
Tower is received further to recycle.
Further, step (1) neutralize acidification in, neutralization be adjusted to pH be 6~7, acid solution be sulphur, carbonic acid, nitric acid and/
Or hydrochloric acid, acid solution molar concentration >=1mol/L.
Further, in step (2) purification by liquid extraction, crude acrylic acid N-butyl is as extractant, extractant additional amount and mixed
The mass ratio for closing waste water is 1:3~1:10, and crude acrylic acid N-butyl is that the content that device generates is more than 95% crude product, and extracts
It takes containing polymerization inhibitor in agent, the extraction residence time is 2~10min.
Further, in step (3) stratification, oil phasor is stablized when keeping standing split-phase, and makes the grease in standing
Split-phase mass ratio is 1:3~1:10.
Further, the polymerization inhibitor be ZJ-701, it is phenthazine, p methoxy phenol, one or two kinds of in hydroquinone
Above mixture；The addition dosage of the polymerization inhibitor are as follows: content in extract liquor is made to maintain 0.02~0.04wt%.
Embodiment 1
The invention discloses drop COD processing unit, including butyl acrylate reaction kettle, water with waste water in a kind of n-butyl acrylate
Surge tank, phase-splitter, polymerization inhibitor tank, crude acrylic acid N-butyl tank, acid solution tank, forced circulation pump, cyclically charging pump, the water
Surge tank is connected to by mixer with the first feed pipe of the phase-splitter, the butyl acrylate reaction kettle, polymerization inhibitor tank,
Crude acrylic acid N-butyl tank is connected to the second feed pipe simultaneously, and the acid solution tank is connected to the input terminal pipeline of mixer,
The input terminal of the forced circulation pump is connected to the phase-splitter pipeline with output end；The oil of the phase-splitter mutually with it is described strong
The input terminal pipeline of charge pump processed is connected to, and the output end for forcing charge pump is connected to second feed pipe.
In the present embodiment, the waste water output channel of the input terminal of the water surge tank and neutralizing tower, dehydrating tower, lightness-removing column
Connection, the neutralizing tower, dehydrating tower, lightness-removing column pH value of waste water be 8.0~11.0.The butyl acrylate reaction kettle and second
Between feed pipe be equipped with the first control valve, between the acid solution tank and the mixer be equipped with the second control valve, described point
PH sensor is equipped with inside phase device, first control valve, the second control valve are connect with the pH sensor simultaneously.The split-phase
The water phase output end of device is connected to Sewage treatment tower tube road.The phase-splitter is the phase-splitter with partition.
Another aspect of the present invention is the waste water drop COD treatment process disclosed using above-mentioned wastewater treatment equipment,
The following steps are included:
(1) it neutralizes acidification: alkaline water technique waste water is mixed to neutralization acidification with acid solution；
2) purification by liquid extraction: crude acrylic acid N-butyl is added in the mixture for neutralizing acidification, and purification by liquid extraction is carried out in phase-splitter；
3) stratification: standing separates oily phase and water phase, and oil is mutually recycled and is returned reaction kettle, and water phase is sent to waste water and returns
Tower is received further to recycle.
In this embodiment, step (1) neutralizes in acidification, and it is 6~7 that neutralization, which is adjusted to pH, and acid solution is sulfuric acid, carbonic acid, nitre
Acid and/or hydrochloric acid, acid solution molar concentration >=1mol/L；In step (2) purification by liquid extraction, crude acrylic acid N-butyl is as extraction
The mass ratio of agent, extractant additional amount and composite waste is 1:10, and crude acrylic acid N-butyl is that the content that device generates is more than 95%
Crude product, and in extractant contain polymerization inhibitor, the extraction residence time be 6min；In step (3) stratification, keep standing split-phase
When oil phasor stablize, and make stand in grease split-phase mass ratio 1:3；The polymerization inhibitor is ZJ-701；The polymerization inhibitor
Dosage is added are as follows: content in extract liquor is made to maintain 0.02~0.04wt%.
Embodiment 2
The invention discloses drop COD processing unit, including butyl acrylate reaction kettle, water with waste water in a kind of n-butyl acrylate
Surge tank, phase-splitter, polymerization inhibitor tank, crude acrylic acid N-butyl tank, acid solution tank, forced circulation pump, cyclically charging pump, the water
Surge tank is connected to by mixer with the first feed pipe of the phase-splitter, the butyl acrylate reaction kettle, polymerization inhibitor tank,
Crude acrylic acid N-butyl tank is connected to the second feed pipe simultaneously, and the acid solution tank is connected to the input terminal pipeline of mixer,
The input terminal of the forced circulation pump is connected to the phase-splitter pipeline with output end；The oil of the phase-splitter mutually with it is described strong
The input terminal pipeline of charge pump processed is connected to, and the output end for forcing charge pump is connected to second feed pipe.
In the present embodiment, the waste water output channel of the input terminal of the water surge tank and neutralizing tower, dehydrating tower, lightness-removing column
Connection, the neutralizing tower, dehydrating tower, lightness-removing column pH value of waste water be 8.0~11.0.The butyl acrylate reaction kettle and second
Between feed pipe be equipped with the first control valve, between the acid solution tank and the mixer be equipped with the second control valve, described point
PH sensor is equipped with inside phase device, first control valve, the second control valve are connect with the pH sensor simultaneously.The split-phase
The water phase output end of device is connected to Sewage treatment tower tube road.The phase-splitter is the phase-splitter with partition.
Another aspect of the present invention is the waste water drop COD treatment process disclosed using above-mentioned wastewater treatment equipment,
The following steps are included:
(1) it neutralizes acidification: alkaline water technique waste water is mixed to neutralization acidification with acid solution；
2) purification by liquid extraction: crude acrylic acid N-butyl is added in the mixture for neutralizing acidification, and purification by liquid extraction is carried out in phase-splitter；
3) stratification: standing separates oily phase and water phase, and oil is mutually recycled and is returned reaction kettle, and water phase is sent to waste water and returns
Tower is received further to recycle.
In this embodiment, step (1) neutralizes in acidification, and it is 6~7 that neutralization, which is adjusted to pH, and acid solution is sulphur, carbonic acid, nitric acid
And/or hydrochloric acid, acid solution molar concentration >=1mol/L；In step (2) purification by liquid extraction, crude acrylic acid N-butyl as extractant,
The mass ratio of extractant additional amount and composite waste be 1:7, crude acrylic acid N-butyl be device generate content be more than 95% it is thick
Product, and contain polymerization inhibitor in extractant, the extraction residence time is 2min；In step (3) stratification, oil when keeping standing split-phase
Phasor is stablized, and makes the grease split-phase mass ratio 1:10 in standing；The polymerization inhibitor is phenthazine, p methoxy phenol；Institute
State the addition dosage of polymerization inhibitor are as follows: content in extract liquor is made to maintain 0.02~0.04wt%.
Embodiment 3
The invention discloses drop COD processing unit, including butyl acrylate reaction kettle, water with waste water in a kind of n-butyl acrylate
Surge tank, phase-splitter, polymerization inhibitor tank, crude acrylic acid N-butyl tank, acid solution tank, forced circulation pump, cyclically charging pump, the water
Surge tank is connected to by mixer with the first feed pipe of the phase-splitter, the butyl acrylate reaction kettle, polymerization inhibitor tank,
Crude acrylic acid N-butyl tank is connected to the second feed pipe simultaneously, and the acid solution tank is connected to the input terminal pipeline of mixer,
The input terminal of the forced circulation pump is connected to the phase-splitter pipeline with output end；The oil of the phase-splitter mutually with it is described strong
The input terminal pipeline of charge pump processed is connected to, and the output end for forcing charge pump is connected to second feed pipe.
In the present embodiment, the waste water output channel of the input terminal of the water surge tank and neutralizing tower, dehydrating tower, lightness-removing column
Connection, the neutralizing tower, dehydrating tower, lightness-removing column pH value of waste water be 8.0~11.0.The butyl acrylate reaction kettle and second
Between feed pipe be equipped with the first control valve, between the acid solution tank and the mixer be equipped with the second control valve, described point
PH sensor is equipped with inside phase device, first control valve, the second control valve are connect with the pH sensor simultaneously.The split-phase
The water phase output end of device is connected to Sewage treatment tower tube road.The phase-splitter is the phase-splitter with partition.
Another aspect of the present invention is the waste water drop COD treatment process disclosed using above-mentioned wastewater treatment equipment,
The following steps are included:
(1) it neutralizes acidification: alkaline water technique waste water is mixed to neutralization acidification with acid solution；
2) purification by liquid extraction: crude acrylic acid N-butyl is added in the mixture for neutralizing acidification, and purification by liquid extraction is carried out in phase-splitter；
3) stratification: standing separates oily phase and water phase, and oil is mutually recycled and is returned reaction kettle, and water phase is sent to waste water and returns
Tower is received further to recycle.
In this embodiment, step (1) neutralizes in acidification, and it is 6~7 that neutralization, which is adjusted to pH, and acid solution is sulphur, carbonic acid, nitric acid
And/or hydrochloric acid, acid solution molar concentration >=1mol/L；In step (2) purification by liquid extraction, crude acrylic acid N-butyl as extractant,
The mass ratio of extractant additional amount and composite waste be 1:3, crude acrylic acid N-butyl be device generate content be more than 95% it is thick
Product, and contain polymerization inhibitor in extractant, the extraction residence time is 10min；In step (3) stratification, when keeping standing split-phase
Oily phasor is stablized, and makes the grease split-phase mass ratio 1:7 in standing；The polymerization inhibitor is hydroquinone；The polymerization inhibitor
Dosage is added are as follows: content in extract liquor is made to maintain 0.02~0.04wt%.
Embodiment 4
The invention discloses drop COD processing unit, including butyl acrylate reaction kettle, water with waste water in a kind of n-butyl acrylate
Surge tank, phase-splitter, polymerization inhibitor tank, crude acrylic acid N-butyl tank, acid solution tank, forced circulation pump, cyclically charging pump, the water
Surge tank is connected to by mixer with the first feed pipe of the phase-splitter, the butyl acrylate reaction kettle, polymerization inhibitor tank,
Crude acrylic acid N-butyl tank is connected to the second feed pipe simultaneously, and the acid solution tank is connected to the input terminal pipeline of mixer,
The input terminal of the forced circulation pump is connected to the phase-splitter pipeline with output end；The oil of the phase-splitter mutually with it is described strong
The input terminal pipeline of charge pump processed is connected to, and the output end for forcing charge pump is connected to second feed pipe.
In the present embodiment, the waste water output channel of the input terminal of the water surge tank and neutralizing tower, dehydrating tower, lightness-removing column
Connection, the neutralizing tower, dehydrating tower, lightness-removing column pH value of waste water be 8.0~11.0.The butyl acrylate reaction kettle and second
Between feed pipe be equipped with the first control valve, between the acid solution tank and the mixer be equipped with the second control valve, described point
PH sensor is equipped with inside phase device, first control valve, the second control valve are connect with the pH sensor simultaneously.The split-phase
The water phase output end of device is connected to Sewage treatment tower tube road.The phase-splitter is the phase-splitter with partition.
Another aspect of the present invention is the waste water drop COD treatment process disclosed using above-mentioned wastewater treatment equipment,
The following steps are included:
(1) it neutralizes acidification: alkaline water technique waste water is mixed to neutralization acidification with acid solution；
2) purification by liquid extraction: crude acrylic acid N-butyl is added in the mixture for neutralizing acidification, and purification by liquid extraction is carried out in phase-splitter；Mixing
After extraction, part mixed liquor is transferred to the phase-splitter other side, is stood, and makes complete split-phase；
3) stratification: standing separates oily phase and water phase, and oil is mutually recycled and is returned reaction kettle, and water phase is sent to waste water and returns
Tower is received further to recycle.
In this embodiment, step (1) neutralizes in acidification, and it is 6~7 that neutralization, which is adjusted to pH, to be neutral to faintly acid, acid solution
For sulphur, carbonic acid, nitric acid and/or hydrochloric acid, acid solution molar concentration >=1mol/L, it is also possible to use resin cation adjusting
PH value；In step (2) purification by liquid extraction, crude acrylic acid N-butyl is as extractant, the quality of extractant additional amount and composite waste
Than for 1:10, crude acrylic acid N-butyl is the crude product that the content that device generates is more than 95%, and containing polymerization inhibitor, extraction in extractant
Taking the residence time is 4min；In step (3) stratification, oil phasor is stablized when keeping standing split-phase, and makes the grease in standing
Split-phase mass ratio is 1:5；The polymerization inhibitor is the mixture of ZJ-701, phenthazine, p methoxy phenol, hydroquinone；It is described
The addition dosage of polymerization inhibitor are as follows: content in extract liquor is made to maintain 0.02~0.04wt%.
Embodiment 5
The invention discloses drop COD processing unit, including butyl acrylate reaction kettle, water with waste water in a kind of n-butyl acrylate
Surge tank, phase-splitter, polymerization inhibitor tank, crude acrylic acid N-butyl tank, acid solution tank, forced circulation pump, cyclically charging pump, the water
Surge tank is connected to by mixer with the first feed pipe of the phase-splitter, the butyl acrylate reaction kettle, polymerization inhibitor tank,
Crude acrylic acid N-butyl tank is connected to the second feed pipe simultaneously, and the acid solution tank is connected to the input terminal pipeline of mixer,
The input terminal of the forced circulation pump is connected to the phase-splitter pipeline with output end；The oil of the phase-splitter mutually with it is described strong
The input terminal pipeline of charge pump processed is connected to, and the output end for forcing charge pump is connected to second feed pipe.
In the present embodiment, the waste water output channel of the input terminal of the water surge tank and neutralizing tower, dehydrating tower, lightness-removing column
Connection, the neutralizing tower, dehydrating tower, lightness-removing column pH value of waste water be 8.0~11.0.The butyl acrylate reaction kettle and second
Between feed pipe be equipped with the first control valve, between the acid solution tank and the mixer be equipped with the second control valve, described point
PH sensor is equipped with inside phase device, first control valve, the second control valve are connect with the pH sensor simultaneously.The split-phase
The water phase output end of device is connected to Sewage treatment tower tube road.The phase-splitter is the phase-splitter with partition.
Another aspect of the present invention is the waste water drop COD treatment process disclosed using above-mentioned wastewater treatment equipment,
The following steps are included:
(1) it neutralizes acidification: alkaline water technique waste water is mixed to neutralization acidification with acid solution；
2) purification by liquid extraction: crude acrylic acid N-butyl is added in the mixture for neutralizing acidification, and purification by liquid extraction is carried out in phase-splitter；
3) stratification: standing separates oily phase and water phase, and oil is mutually recycled and is returned reaction kettle, and water phase is sent to waste water and returns
Tower is received further to recycle.
In this embodiment, step (1) neutralizes in acidification, and it is 6~7 that neutralization, which is adjusted to pH, and acid solution is sulphur, carbonic acid, nitric acid
And/or hydrochloric acid, acid solution molar concentration >=1mol/L；In step (2) purification by liquid extraction, crude acrylic acid N-butyl as extractant,
The mass ratio of extractant additional amount and composite waste be 1:8, crude acrylic acid N-butyl be device generate content be more than 95% it is thick
Product, and contain polymerization inhibitor in extractant, the extraction residence time is 7min；In step (3) stratification, oil when keeping standing split-phase
Phasor is stablized, and makes the grease split-phase mass ratio 1:7 in standing；The polymerization inhibitor is ZJ-701, phenthazine；The polymerization inhibitor
Addition dosage are as follows: so that content is maintained 0.02~0.04wt%.
Application Example 1
In producing 100000 tons of butyl acrylate device per year, original process device water surge tank (waste water from neutralizing tower, dehydrating tower and
Lightness-removing column) alkaline waste water (5.36m that is continuously discharged3/ h), it is mixed by mixer with the sulfuric acid of 1M, passes through control valve and split-phase
PH sensors association controls in device, and keeping pH in analyzer is 6, and the connected pump of phase-splitter carries out the mixture of phase-splitter side
Forced circulation, and butyl acrylate is added and is extracted, makes to extract oil-water ratio and maintains near 1:3, extracts the residence time and is
5min.Mixed liquor carries out two sections of standing split-phases of junior, and (flow is 5.15 m to aqueous portion3/ h) it is sent to the progress of Sewage treatment tower most
Recycling afterwards, mutually a part is used as extractant to oil, and a part sends to reaction kettle.Waste water COD is finally discharged in Sewage treatment tower
21600mg/L, flow are 4.43 m3/h。
Application Example 2
In producing 100000 tons of butyl acrylate device per year, original process device water surge tank (waste water from neutralizing tower, dehydrating tower and
Lightness-removing column) alkaline waste water (5.36m that is continuously discharged3/ h), it is mixed by mixer with the sulfuric acid of 1M, passes through control valve and split-phase
PH sensors association controls in device, and keeping pH in analyzer is 6.8, the connected pump of phase-splitter to the mixture of phase-splitter side into
Row forced circulation, and butyl acrylate is added and is extracted, it maintains extraction oil-water ratio near 1:8, extracts the residence time
For 3min.Mixed liquor carries out two sections of standing split-phases of junior, and (flow is 5.20 m to aqueous portion3/ h) it is sent to the progress of Sewage treatment tower
Last recycling, mutually a part is used as extractant to oil, and a part sends to reaction kettle.Waste water COD is finally discharged in Sewage treatment tower
28300mg/L, flow are 4.50 m3/h。
Application Example 3
In producing 100000 tons of butyl acrylate device per year, original process device water surge tank (waste water from neutralizing tower, dehydrating tower and
Lightness-removing column) alkaline waste water (5.36m that is continuously discharged3/ h), it is fixed with the neutralization reaction pipe (mixer) of resin cation, is passed through
PH sensors association controls in control valve and phase-splitter, and keeping pH in analyzer is 7.0(after cation failure, carries out weight
It is raw), the connected pump of phase-splitter carries out forced circulation to the mixture of phase-splitter side, and butyl acrylate is added and is extracted,
Maintain extraction oil-water ratio near 1:3, the extraction residence time is 4min.Mixed liquor carries out two sections of standing split-phases of junior, water
Mutually (flow is 5.25 m for part3/ h) it is sent to Sewage treatment tower and carries out last recycling, mutually a part is used as extractant to oil, and one
Send dereaction kettle.It is 33300mg/L that waste water COD, which is finally discharged, in Sewage treatment tower, and flow is 4.59 m3/h。
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the present invention in any form；It is all
The those of ordinary skill of the industry can be shown in by specification and described above and swimmingly implement the present invention；But it is all familiar
Professional and technical personnel without departing from the scope of the present invention, makes using disclosed above technology contents
A little variation, modification and evolution equivalent variations, be equivalent embodiment of the invention；Meanwhile all realities according to the present invention
The variation, modification and evolution etc. of matter technology any equivalent variations to the above embodiments, still fall within technology of the invention
Within the protection scope of scheme.
Claims (10)
1. in a kind of n-butyl acrylate and waste water drop COD processing unit, including butyl acrylate reaction kettle, water surge tank, point
Phase device, polymerization inhibitor tank, crude acrylic acid N-butyl tank, the water surge tank pass through the first feed pipe of mixer and the phase-splitter
Road connection, the butyl acrylate reaction kettle, polymerization inhibitor tank, crude acrylic acid N-butyl tank are connected to the second feed pipe simultaneously,
It is characterized by also including acid solution tank, forced circulation pump, cyclically charging pump, the input terminals of the acid solution tank and mixer
Pipeline connection, the input terminal of the forced circulation pump are connected to the phase-splitter pipeline with output end；The oil of the phase-splitter
It is mutually connected to the input terminal pipeline for forcing charge pump, the output end for forcing charge pump and second feed pipe connect
It is logical.
2. in n-butyl acrylate according to claim 1 and COD processing unit drops in waste water, it is characterised in that: the water
The input terminal of surge tank is connected to the waste water output channel of neutralizing tower, dehydrating tower, lightness-removing column, and the neutralizing tower, takes off gently dehydrating tower
The pH value of waste water of tower is 8.0~11.0.
3. in n-butyl acrylate according to claim 2 and COD processing unit drops in waste water, it is characterised in that: described third
It is equipped with the first control valve between olefin(e) acid butyl ester reaction kettle and the second feed pipe, is set between the acid solution tank and the mixer
There is the second control valve, is equipped with pH sensor inside the phase-splitter, second control valve is connect with the pH sensor simultaneously.
4. in n-butyl acrylate according to claim 3 and COD processing unit drops in waste water, it is characterised in that: described point
The water phase output end of phase device is connected to Sewage treatment tower tube road.
5. in n-butyl acrylate according to claim 4 and COD processing unit drops in waste water, it is characterised in that: described point
Phase device is the phase-splitter with partition.
6. COD treatment process drops in a kind of waste water using wastewater treatment equipment described in Claims 1 to 55, it is characterised in that including
Following steps:
(1) it neutralizes acidification: alkaline water technique waste water is mixed to neutralization acidification with acid solution；
2) purification by liquid extraction: crude acrylic acid N-butyl is added in the mixture for neutralizing acidification, and purification by liquid extraction is carried out in phase-splitter；
3) stratification: standing separates oily phase and water phase, and oil is mutually recycled and is returned reaction kettle, and water phase is sent to waste water and returns
Tower is received further to recycle.
7. COD treatment process drops in waste water according to claim 6, it is characterised in that: step (1) neutralizes in acidification, neutralizes
Being adjusted to pH is 6~7, and acid solution is sulfuric acid, carbonic acid, nitric acid and/or hydrochloric acid, acid solution molar concentration >=1mol/L.
8. COD treatment process drops in waste water according to claim 7, it is characterised in that: in step (2) purification by liquid extraction, thick third
For olefin(e) acid N-butyl as extractant, the mass ratio of extractant additional amount and composite waste is 1:3~1:10, crude acrylic acid N-butyl
Be device generate content be more than 95% crude product, and in extractant contain polymerization inhibitor, the extraction residence time be 2~10min.
9. COD treatment process drops in waste water according to claim 8, it is characterised in that: in step (3) stratification, keep
Oil phasor is stablized when standing split-phase, and makes grease split-phase mass ratio 1:3~1:10 in standing.
10. COD treatment process drops in waste water according to claim 9, it is characterised in that: the polymerization inhibitor is ZJ-701, pheno
Thiazine, p methoxy phenol, mixture one or more kinds of in hydroquinone；The addition dosage of the polymerization inhibitor are as follows: make
Content maintains 0.02~0.04wt% in extract liquor.
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| CN110357272A (en) * | 2019-07-19 | 2019-10-22 | 江门谦信化工发展有限公司 | A kind for the treatment of process applied to acrylic acid and esters of acrylic acid waste water |
| CN114230072A (en) * | 2021-11-30 | 2022-03-25 | 江苏三木化工股份有限公司 | Efficient treatment method of acrylate monomer wastewater |
| CN115490590A (en) * | 2022-08-29 | 2022-12-20 | 平湖石化有限责任公司 | Butyl acrylate continuous production process with acrylic acid circulation |
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