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CN111892118A - Extraction process of phenol-containing wastewater of sebacic acid production device - Google Patents

Extraction process of phenol-containing wastewater of sebacic acid production device Download PDF

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Publication number
CN111892118A
CN111892118A CN202010913895.3A CN202010913895A CN111892118A CN 111892118 A CN111892118 A CN 111892118A CN 202010913895 A CN202010913895 A CN 202010913895A CN 111892118 A CN111892118 A CN 111892118A
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extractant
tank
extraction
pump
opening
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吴自胜
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Shandong Chiyue Chemical Co ltd
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Shandong Chiyue Chemical Co ltd
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    • 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
    • C02F1/26Treatment of water, waste water, or sewage by extraction
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/34Organic compounds containing oxygen
    • C02F2101/345Phenols
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2303/00Specific treatment goals
    • C02F2303/18Removal of treatment agents after treatment

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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)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a process for extracting phenol-containing wastewater of a sebacic acid production device, which comprises the steps of extraction, back extraction and acid washing, wherein the extraction, the back extraction and the acid washing are sequentially carried out according to the operations of the extraction, the back extraction and the acid washing, and the extraction comprises the following steps: s1, starting a storage tank delivery pump of the extractant N-503, sending the N-503 to an extractant 2# tank, and closing the delivery pump after the extractant 2# tank reaches the liquid level; s2, starting the wastewater delivery pump, opening an outlet valve of the delivery pump, adjusting an inlet valve of the rotameter, and slowly adjusting the flow of the wastewater to a specified flow of 20m 3/h; the device has a scientific and reasonable structure, is safe and convenient to use, adopts N-503 (chemical name: N, N-di (1-methylheptyl) acetamide) as an extracting agent, has excellent extraction selectivity, adopts an extractor for extraction in extraction equipment and back extraction equipment, adopts three-stage extraction for extraction, adopts two-stage back extraction for back extraction, has an extraction rate of 95-99 percent, occupies a small area, and can completely recycle the extracted phenol into a production system.

Description

Extraction process of phenol-containing wastewater of sebacic acid production device
Technical Field
The invention relates to the technical field of wastewater extraction of a sebacic acid production device, in particular to a phenol-containing wastewater extraction process of the sebacic acid production device.
Background
According to the domestic sebacic acid production method, castor oil is hydrolyzed to generate ricinoleic acid, the ricinoleic acid and phenol (serving as a diluent and a catalyst) are subjected to pyrolysis to obtain sebacic acid disodium salt, and the sebacic acid disodium salt is neutralized, acidified and crystallized to obtain a product sebacic acid, but a large amount of phenol-containing wastewater is generated in the production, about 20-30 tons of phenol-containing wastewater is generated in the production of 1 ton of sebacic acid, the pH value is 2-3, the phenol mass concentration is 4000-5000 mg/l, the COD (chemical oxygen demand) reaches 20000mg/l, and the sebacic acid disodium salt also contains about 7-8% of sodium sulfate, and belongs to high-salt phenol-containing wastewater;
at present, manufacturers adopt secondary octanol which is a byproduct in sebacic acid production as an extracting agent, and extract the secondary octanol by using an extraction tower, wherein the extraction rate is 90-95%, and the defects are that the occupied area is large, and the secondary octanol after back extraction contains a small amount of phenol and influences the later application of the secondary octanol.
Disclosure of Invention
The invention provides a phenol-containing wastewater extraction process of a sebacic acid production device, which can effectively solve the problems that the existing manufacturers adopt secondary octanol which is a byproduct of sebacic acid production as an extraction agent, the extraction rate is 90-95% by using an extraction tower for extraction, the occupied area is large, the secondary octanol contains a small amount of phenol after back extraction, and the influence is caused on the later-stage application of the secondary octanol in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: the extraction process of the phenol-containing wastewater of the sebacic acid production device comprises extraction, acid washing and back extraction, and the extraction, the back extraction and the acid washing are sequentially carried out.
According to the technical scheme, the extraction comprises the following steps:
s1, starting a storage tank delivery pump of the extractant N-503, sending the N-503 to an extractant 2# tank, and closing the delivery pump after the extractant 2# tank reaches the liquid level;
s2, starting the wastewater delivery pump, opening the outlet valve of the delivery pump, adjusting the inlet valve of the rotameter, and slowly adjusting the wastewater flow to the specified flow of 20m3/h;
S3, when the waste water flow is observed from the plastic transparent tube, starting the extractant pump, opening the outlet valve of the pump, adjusting the inlet valve of the rotameter to a proper flow rate of 3m3/h;
S4, when the extractant flows out of the transparent plastic pipe, starting an extractant circulating pump, opening an outlet valve of the circulating pump, sending the extractant into an extractant 3# tank, opening an outlet valve at the bottom of the extractant 3# tank, closing the outlet valve at the bottom of the extractant 2# tank, simultaneously opening an extractant inlet valve at the upper part of the extractant 2# tank, and enabling the extractant to enter the extractant 2# tank;
s5, when the extractant 3# tank reaches a low-level liquid level alarm, opening the bottom outlet valve of the extractant 2# tank, closing the bottom outlet valve of the extractant 3# tank, opening the upper inlet valve of the extractant 4# tank, closing the upper inlet valve of the extractant 2# tank, simultaneously starting the workshop N-503 storage tank delivery pump, adding N-503 into the extractant 3# tank, when the low-level liquid level alarm of the extractant 2# tank, opening the bottom outlet valve of the extractant 3# tank, closing the bottom outlet valve of the extractant 2# tank, opening the upper inlet valve of the extractant 2# tank, and circulating the steps.
According to the technical scheme, the volume of the extractant 2# tank in the S1 is 20m3 after reaching the liquid level;
the time for alarming when the liquid level of the extractant 2# tank in the S2 reaches a low level is 6 hours;
the time for alarming when the extraction agent 3# tank reaches a low liquid level is 6 hours;
and the low-level liquid level of the extractant 2# tank alarms for 6 hours.
According to the technical scheme, the pickling comprises the following steps:
s1, adding tap water into an acid preparation tank according to a certain flow, and then adding a certain amount of concentrated sulfuric acid to prepare a dilute sulfuric acid solution;
s2, opening an outlet valve at the bottom of an extractant 4# tank, starting an extractant pickling pump, adjusting the flow rate, sequentially adding the extractant into a pickling tank, starting a dilute acid pump, adding dilute acid into the pickling tank, separating the dilute acid into a dilute acid treatment tank, separating N-503, sending the N-503 into the extractant 2# tank or the extractant 3# tank by using a pickling recovery pump, and carrying out next pickling.
According to the technical scheme, the flow of tap water in the S1 is 15M3/h;
In the step S2, the flow is adjusted to be 20min, and the volume is 2m3
The control flow rate in S2 is 2.5m3H for 10-15min, and 0.5m in total3Acid washing, stirring for 10-15min, stopping stirring, standing for 30min, and separating out diluted acid to dilute acid treatment tank.
According to the technical scheme, the back extraction comprises the following steps:
s1, starting a crude alkali pump, adding 30% liquid alkali into the prepared alkali through a flow meterIn a tank, then add water 2.5m through a flow meter3Preparing an alkaline water solution;
s2, starting the alkali stripping pump, opening an outlet valve of the alkali stripping pump, and regulating the flow of the liquid alkali to the specified flow of 0.6m through a liquid alkali flow meter3Adding the prepared liquid alkali into the extractor, starting the extractant back-extraction pump when the liquid alkali is seen from the transparent plastic pipe, opening the outlet valve of the pump, adjusting the flow of the treated extractant, and controlling the flow of the flow meter to be 2.4m3Performing back extraction;
s3, feeding the back-extracted liquid caustic soda into a sodium phenolate receiving tank, pumping the liquid caustic soda into a cracking process, preparing 48% liquid caustic soda by using solid caustic soda, and feeding the liquid caustic soda into a cracking kettle;
and S4, feeding the back-extracted extractant into an extractant No. 2 tank or a No. 3 tank, and continuing to extract.
According to the technical scheme, the volume of the alkali preparation tank is 2.5m3
The concentration of the aqueous alkali solution is 15-20%.
Compared with the prior art, the invention has the beneficial effects that: the device has a scientific and reasonable structure, is safe and convenient to use, adopts N-503 (chemical name: N, N-di (1-methylheptyl) acetamide) as an extracting agent, has excellent extraction selectivity, adopts an extractor for extraction in extraction equipment and back extraction equipment, adopts three-stage extraction for extraction, adopts two-stage back extraction for back extraction, has an extraction rate of 95-99 percent, occupies a small area, and can completely recycle the extracted phenol into a production system.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention.
In the drawings:
FIG. 1 is a schematic diagram of an extraction scheme according to the present invention;
FIG. 2 is a schematic diagram of the pickling process of the present invention;
FIG. 3 is a schematic diagram of a stripping process according to the present invention;
FIG. 4 is a schematic diagram of the processing system of the present invention.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
Example (b): as shown in figures 1-4, the invention provides a technical scheme that a sebacic acid production device phenol-containing wastewater extraction process comprises extraction, acid washing and back extraction, and the operations of the extraction, the acid washing and the back extraction are sequentially carried out.
According to the technical scheme, the extraction comprises the following steps:
s1, starting a storage tank delivery pump of the extractant N-503, sending the N-503 to an extractant 2# tank, and closing the delivery pump after the extractant 2# tank reaches the liquid level;
s2, starting the wastewater delivery pump, opening the outlet valve of the delivery pump, adjusting the inlet valve of the rotameter, and slowly adjusting the wastewater flow to the specified flow of 20m3/h;
S3, when the waste water flow is observed from the plastic transparent tube, starting the extractant pump, opening the outlet valve of the pump, adjusting the inlet valve of the rotameter to a proper flow rate of 3m3/h;
S4, when the extractant flows out of the transparent plastic pipe, starting an extractant circulating pump, opening an outlet valve of the circulating pump, sending the extractant into an extractant 3# tank, opening an outlet valve at the bottom of the extractant 3# tank, closing the outlet valve at the bottom of the extractant 2# tank, simultaneously opening an extractant inlet valve at the upper part of the extractant 2# tank, and enabling the extractant to enter the extractant 2# tank;
s5, when the extractant 3# tank reaches a low-level liquid level alarm, opening the bottom outlet valve of the extractant 2# tank, closing the bottom outlet valve of the extractant 3# tank, opening the upper inlet valve of the extractant 4# tank, closing the upper inlet valve of the extractant 2# tank, simultaneously starting the workshop N-503 storage tank delivery pump, adding N-503 into the extractant 3# tank, when the low-level liquid level alarm of the extractant 2# tank, opening the bottom outlet valve of the extractant 3# tank, closing the bottom outlet valve of the extractant 2# tank, opening the upper inlet valve of the extractant 2# tank, and circulating the steps.
According to the technical scheme, the volume of the extractant 2# tank in the S1 is about 20m after the liquid level is reached3
When the liquid level of the extractant 2# tank in the S2 reaches a low level, alarming for 6 hours;
the time for alarming when the extraction agent 3# tank reaches a low level liquid level is 6 hours;
the time for alarming the low-level liquid level of the extractant 2# tank is 6 hours.
According to the technical scheme, the pickling comprises the following steps:
s1, adding tap water into an acid preparation tank according to a certain flow, and then adding a certain amount of concentrated sulfuric acid to prepare a dilute sulfuric acid solution;
s2, opening an outlet valve at the bottom of an extractant 4# tank, starting an extractant pickling pump, adjusting the flow rate, sequentially adding the extractant into a pickling tank, starting a dilute acid pump, adding dilute acid into the pickling tank, separating the dilute acid into a dilute acid treatment tank, separating N-503, sending the N-503 into the extractant 2# tank or the extractant 3# tank by using a pickling recovery pump, and carrying out next pickling.
According to the technical scheme, the flow of tap water in S1 is 15M3/h;
In S2, the flow rate is adjusted to 20min, and the volume is about 2m3
Control flow 2.5m in S23H for 12min, total 0.5m3Acid washing, stirring for 13min, stopping stirring, standing for 30min, and separating out dilute acid in a dilute acid treatment tank.
According to the technical scheme, the back extraction comprises the following steps:
s1, starting a crude alkali pump, adding 30% liquid alkali into an alkali preparation tank through a flow meter, and adding 2.5m of water through the flow meter3Preparing an alkaline water solution;
s2, starting the alkali stripping pump, opening an outlet valve of the alkali stripping pump, and regulating the flow of the liquid alkali to the specified flow of 0.6m through a liquid alkali flow meter3H, adding the prepared liquid alkali into an extractorWhen liquid alkali is seen in the transparent plastic pipe, the extractant back-extraction pump is started, the outlet valve of the pump is opened, the flow of the treated extractant is regulated, and the flow of the control flowmeter is 2.4m3Performing back extraction;
s3, feeding the back-extracted liquid caustic soda into a sodium phenolate receiving tank, pumping the liquid caustic soda into a cracking process, preparing 48% liquid caustic soda by using solid caustic soda, and feeding the liquid caustic soda into a cracking kettle;
and S4, feeding the back-extracted extractant into an extractant No. 2 tank or a No. 3 tank, and continuing to extract.
According to the technical scheme, the volume of the alkali preparation tank is 2.5m3
The concentration of the aqueous alkali solution is 18 percent.
Compared with the prior art, the invention has the beneficial effects that: the device has a scientific and reasonable structure, is safe and convenient to use, adopts N-503 (chemical name: N, N-di (1-methylheptyl) acetamide) as an extracting agent, has excellent extraction selectivity, adopts an extractor for extraction in extraction equipment and back extraction equipment, adopts three-stage extraction for extraction, adopts two-stage back extraction for back extraction, has an extraction rate of 95-99 percent, occupies a small area, and can completely recycle the extracted phenol into a production system.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (7)

1. The extraction process of phenol-containing wastewater of a sebacic acid production device is characterized by comprising the following steps of: comprises extraction, back extraction and acid washing, and the operations of extraction, acid washing and back extraction are carried out in sequence.
2. The extraction process of phenol-containing wastewater of sebacic acid production plant according to claim 1, characterized in that the extraction comprises the steps of:
s1, starting a storage tank delivery pump of the extractant N-503, sending the N-503 to an extractant 2# tank, and closing the delivery pump after the extractant 2# tank reaches the liquid level;
s2, starting the wastewater delivery pump, opening an outlet valve of the delivery pump, adjusting an inlet valve of a rotor flow meter, and slowly adjusting the flow of the wastewater to the specified flow of 20m3/h;
S3, when the waste water flow is observed from the plastic transparent tube, starting the extractant pump, opening the outlet valve of the pump, adjusting the inlet valve of the rotameter to a proper flow rate of 3m3/h;
S4, when the extractant flows out of the transparent plastic pipe, starting an extractant circulating pump, opening an outlet valve of the circulating pump, sending the extractant into an extractant 3# tank, opening an outlet valve at the bottom of the extractant 3# tank, closing the outlet valve at the bottom of the extractant 2# tank, simultaneously opening an extractant inlet valve at the upper part of the extractant 2# tank, and enabling the extractant to enter the extractant 2# tank;
s5, when the extractant 3# tank reaches a low-level liquid level alarm, opening the bottom outlet valve of the extractant 2# tank, closing the bottom outlet valve of the extractant 3# tank, opening the upper inlet valve of the extractant 4# tank, closing the upper inlet valve of the extractant 2# tank, simultaneously starting the workshop N-503 storage tank delivery pump, adding N-503 into the extractant 3# tank, when the low-level liquid level alarm of the extractant 2# tank, opening the bottom outlet valve of the extractant 3# tank, closing the bottom outlet valve of the extractant 2# tank, opening the upper inlet valve of the extractant 2# tank, and circulating the steps.
3. The extraction process of phenolic wastewater in a sebacic acid production device according to claim 2, characterized in that the extractant 2# tank in the S1 reaches a liquid level with a volume of 20m3
The time for alarming when the liquid level of the extractant 2# tank in the S2 reaches a low level is 6 hours;
the time for alarming when the extraction agent 3# tank reaches a low liquid level is 6 hours;
and the low-level liquid level of the extractant 2# tank alarms for 6 hours.
4. The extraction process of phenol-containing wastewater of sebacic acid production plant according to claim 1, characterized in that the acid washing comprises the steps of:
s1, adding tap water into an acid preparation tank according to a certain flow, and then adding a certain amount of concentrated sulfuric acid to prepare a dilute sulfuric acid solution;
s2, opening an outlet valve at the bottom of an extractant 4# tank, starting an extractant pickling pump, adjusting the flow rate, sequentially adding the extractant into a pickling tank, starting a dilute acid pump, adding dilute acid into the pickling tank, separating the dilute acid into a dilute acid treatment tank, separating N-503, sending the N-503 into the extractant 2# tank or the extractant 3# tank by using a pickling recovery pump, and carrying out next pickling.
5. The extraction process of phenolic wastewater from sebacic acid production device according to claim 4, wherein tap water in S1 is at a flow rate of 15m 3/h;
in the step S2, the flow is adjusted to be 20min and is 2m in total3
The control flow rate in S2 is 2.5m3H for 10-15min, and 0.5m in total3Acid washing, stirring for 10-15min, stopping stirring, standing for 30min, and separating out diluted acid to dilute acid treatment tank.
6. The extraction process of phenol-containing wastewater of sebacic acid production plant according to claim 1, wherein the stripping comprises the steps of:
s1, starting a crude alkali pump, adding 30% liquid alkali into an alkali preparation tank through a flow meter, and adding 2.5m of water through the flow meter3Preparing an alkaline water solution;
s2, starting the alkali stripping pump, opening an outlet valve of the alkali stripping pump, and regulating the flow of the liquid alkali to the specified flow of 0.6m through a liquid alkali flow meter3Adding the prepared liquid alkali into the extractor, starting the extractant back-extraction pump when the liquid alkali is seen from the transparent plastic pipe, and opening the pump outletA valve for regulating the flow of the extractant to 2.4m3Performing back extraction;
s3, feeding the back-extracted liquid caustic soda into a sodium phenolate receiving tank, pumping the liquid caustic soda into a cracking process, preparing 48% liquid caustic soda by using solid caustic soda, and feeding the liquid caustic soda into a cracking kettle;
and S4, feeding the back-extracted extractant into an extractant No. 2 tank or a No. 3 tank, and continuing to extract.
7. The extraction process of phenol-containing wastewater of sebacic acid production apparatus according to claim 6, wherein the alkali preparation tank has a volume of 2.5m3
The concentration of the aqueous alkali solution is 15-20%.
CN202010913895.3A 2020-09-02 2020-09-02 Extraction process of phenol-containing wastewater of sebacic acid production device Pending CN111892118A (en)

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Cited By (1)

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