CN110040864A - A kind of recovery method that phosphate discharge liquid is electroplated - Google Patents

A kind of recovery method that phosphate discharge liquid is electroplated Download PDF

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Publication number
CN110040864A
CN110040864A CN201910266579.9A CN201910266579A CN110040864A CN 110040864 A CN110040864 A CN 110040864A CN 201910266579 A CN201910266579 A CN 201910266579A CN 110040864 A CN110040864 A CN 110040864A
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outlet
back extraction
oil separator
extraction
input
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焦伟丽
赵紫君
何辉
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Dongguan Sanrenxing Environmental Technology Co Ltd
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Dongguan Sanrenxing Environmental Technology Co Ltd
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Priority to CN201910266579.9A priority Critical patent/CN110040864A/en
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/16—Oxyacids of phosphorus; Salts thereof
    • C01B25/18—Phosphoric acid
    • C01B25/234—Purification; Stabilisation; Concentration
    • C01B25/237—Selective elimination of impurities
    • C01B25/238—Cationic impurities, e.g. arsenic compounds
    • 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
    • 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
    • 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
    • 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
    • C02F2101/10—Inorganic compounds
    • C02F2101/105—Phosphorus compounds
    • 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
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • 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
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • C02F2101/203—Iron or iron compound
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2301/00—General aspects of water treatment
    • C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

The present invention relates to and field of industrial waste water treatment, and in particular to it is a kind of be electroplated phosphate discharge liquid recovery method, include the following steps: 1) by phosphate discharge liquid after oil separator the first treatment fluid；2) the first treatment fluid is obtained into second processing liquid after the first extraction equipment；3) second processing liquid is obtained into third treatment fluid after the second extraction equipment；4) third treatment fluid obtains fourth process liquid after the first back extraction device；5) fourth process liquid is obtained into the 5th treatment fluid after the second back extraction device；6) the 5th treatment fluid is obtained into the 6th treatment fluid after being stripped oil separator；7) the 6th treatment fluid is obtained into the 7th treatment fluid after concentration；8) the 7th treatment fluid can be recycled after detection is up to standard for production line.It is brought down below 0.1mg/L by iron, aluminium content in the recovery method treated phosphate discharge liquid in the present invention, not only reduce processing cost and can also be back on production line through handling phosphoric acid after the recovery.

Description

A kind of recovery method that phosphate discharge liquid is electroplated
Technical field
The present invention relates to field of industrial waste water treatment, and in particular to a kind of recovery method that phosphate discharge liquid is electroplated.
Background technique
Phosphoric acid is widely used in electroplating industry, and the waste liquid containing a large amount of waste phosphoric acids can be discharged in use process, and (phosphoric acid is useless Liquid), containing impurity such as organic matter, iron, aluminium in this kind of waste liquid, direct emission not only causes serious environmental pollution, but also causes pole The big wasting of resources.Phosphorus is the important indicator of evaluating water quality.When the mass concentration of phosphorus in water body is more than 0.01mg/L, it is possible to Cause the eutrophication of water.Plating phosphate discharge liquid conventional treatment, which is discharged to sewage plant, will consume a large amount of Dephosphorization reagent, and generate and contain The very high hazardous waste of moisture content not only wastes processing cost, also to pay expensive treatment of sludge expense.
Summary of the invention
In order to overcome shortcoming and defect existing in the prior art, it is useless that the purpose of the present invention is to provide a kind of plating phosphoric acid The recovery method of liquid, by iron, aluminium content in the recovery method treated phosphate discharge liquid down to 0.1mg/L hereinafter, not only dropping Low processing cost, and can also be back on production line through handling phosphoric acid after the recovery.
The purpose of the invention is achieved by the following technical solution: a kind of recovery method that phosphate discharge liquid is electroplated, including as follows Step:
1) the first treatment fluid for obtaining the phosphate discharge liquid gathered after oil separator removes the impurity such as organic matter；
2) the first treatment fluid obtained in step 1) is obtained into second processing liquid after the first extraction equipment；
3) second processing liquid obtained in step 2) is obtained into third treatment fluid after the second extraction equipment；
4) third treatment fluid obtained in step 3) is obtained into fourth process liquid after the first back extraction device；
5) fourth process liquid obtained in step 4) is obtained into the 5th treatment fluid after the second back extraction device；
6) the 5th treatment fluid obtained in step 5) is obtained into the 6th treatment fluid after being stripped oil separator；
7) the 6th treatment fluid obtained in step 6) is obtained into the 7th treatment fluid after concentration；
8) final step 7) obtained in the 7th treatment fluid through detect it is up to standard after can be recycled for production line.
Iron, aluminium content in phosphate discharge liquid can be down to by phosphate discharge liquid after the processing of above-mentioned processing method in the present invention 0.1mg/L can also be back on production line hereinafter, not only reduce processing cost through handling phosphoric acid after the recovery, kept away Exempt from conventional treatment and be discharged to sewage plant that a large amount of Dephosphorization reagent will be consumed, and generates the very high hazardous waste of water content, it is not only unrestrained The problem of taking processing cost, also paying expensive treatment of sludge expense.
Preferably, vacuum pressure when step 7) concentration is 7.5-8.5KPa, and thickening temperature is 70-80 DEG C.
Vacuum pressure of the concentration technology to concentration when is produced daily using wet process in step 7) of the present invention strictly to be limited, This operating condition flash distillation chamber operating temp is lower, and line with rubber is non-aging, and line with rubber is not easily to fall off under vacuum conditions, extends flash distillation Room service life is conducive to device long-period stable operation.
Preferably, tricresyl phosphate is added in step 2) and the first extraction equipment described in step 3) and the second extraction equipment Butyl ester extractant.
Tributyl phosphate used has that strong to phosphoric acid extraction ability, selectivity is good, solubility is small etc. in water in the present invention Advantage is the phosphoric acid extraction optimum extractant from phosphate discharge liquid.
Preferably, oil separator described in the step 1) includes the first oil separator and the second oil separator, first oil removal The outlet end in pond is connected with the input end of second oil separator；First extraction equipment described in step 2) is equipped with No.1 import End, No. two input ends, No.1 outlet end and No. two outlet ends, the No.1 input end of first extraction equipment and described second The outlet end of oil separator is connected to；Second extraction equipment described in step 3) is equipped with No.1 input end, No. two input ends, No. three imports End, No. four input ends, No.1 outlet end and No. two outlet ends, the No.1 input end of second extraction equipment and described first The No.1 outlet end of extraction equipment is connected to；No. two of the No.1 outlet end of second extraction equipment and first extraction equipment Input end connection；No. four input ends of second extraction equipment are connected to No. two outlet ends of second extraction equipment.
Phosphate discharge liquid can remove the impurity such as organic matter by the processing of oil separator twice well in step 1) of the present invention, it It, can be efficiently by iron, the aluminium in phosphate discharge liquid by the first extraction equipment and the second extraction equipment cycling extraction in step 2 Equal impurity are separated in organic phase, play the role of removal of impurities, while such connection type avoids extractant entrainment, is effectively saved The dosage of extractant sum improves the quality of recycling product.
First extraction equipment is equipped with No.1 input end, No. two input ends, No.1 outlet end and No. two outlet ends；The Two extraction equipments are equipped with No.1 input end, No. two input ends, No. three input ends, No.1 outlet end and No. two outlet ends；First It is stripped device and is equipped with No.1 input end, No. two input ends, No.1 outlet end and No. two outlet ends；Second back extraction device is set There are No.1 outlet end, No. two outlet ends and No. three outlet ends；The first back extraction oil separator is equipped with No.1 input end and No. two Input end.
Preferably, the first back extraction device described in step 4) is equipped with No.1 input end, No. two input ends, No.1 outlet end And No. two outlet ends, the No.1 input end of the first back extraction device and No. two outlet ends of first extraction equipment connect It is logical；Second back extraction device described in step 5) is equipped with No.1 outlet end, No. two outlet ends and No. three outlet ends, and described second is anti- The input end of extraction equipment is connected to the No.1 outlet end of the first back extraction device；The No.1 of the second back extraction device Outlet end is connected to No. two input ends of the second extraction equipment, No. two outlet ends and described first of the second back extraction device It is stripped No. two input ends connection of device, No. three outlet ends of the second back extraction device and second extraction equipment No. three input end connections；Back extraction oil separator described in step 6) includes the first back extraction oil separator and the second back extraction oil removal Pond, the first back extraction oil separator are equipped with No.1 input end and No. two input ends, and No. two of the first back extraction device go out Mouth end is connected to the No.1 input end of the first back extraction oil separator, No. three outlet ends of the second back extraction device and institute State No. two input ends connection of the first back extraction oil separator, the outlet end of the first back extraction oil separator and second back extraction The input end of oil separator is taken to be connected to.
The present invention handles the third treatment fluid after secondary cycle extraction processing through secondary cycle back extraction again, obtains It can be back to the extractant of extraction and second of extraction for the first time, in addition the part after the second back extraction device is not located completely The phosphate discharge liquid managed can transport to the second extraction equipment and continue cycling through processing, the first back extraction oil separator and the second back extraction Taking oil separator is the organic phase that the oil separator for the phosphoric acid solution that back extraction comes out is extraction, and oil spill here flows to having for following settings Machine phase supply case, feeds the first extraction equipment and the extraction of the second extraction equipment uses.And this connection type avoids back extraction The entrainment of agent is effectively saved the dosage of strippant, improves the quality of recycling product.
Preferably, it is 1.2-1.3 that the examination criteria of the 7th treatment fluid, which is water outlet phosphoric acid specific gravity, in step 8), and phosphoric acid concentration is low In 27.5%, iron, aluminium content are below 0.1mg/L.
Phosphate discharge liquid is after the above method is handled in the present invention, and reaching water outlet phosphoric acid specific gravity is 1.2-1.3, and phosphoric acid concentration is low In 27.5%, iron, aluminium content are below the treatment fluid after the standard of 0.1mg/L and can be back on production line, avoid routine Processing, which is discharged to sewage plant, will consume a large amount of Dephosphorization reagent, and generate the very high hazardous waste of water content, and not only waste is processed into Originally, the problem of also paying expensive treatment of sludge expense.
The beneficial effects of the present invention are: a kind of recovery method that phosphate discharge liquid is electroplated, after recovery method processing Phosphate discharge liquid in iron, aluminium content down to 0.1mg/L hereinafter, not only reduce processing cost, and through handling phosphorus after the recovery Acid can also be back on production line, and a large amount of Dephosphorization reagent will be consumed by avoiding conventional treatment and being discharged to sewage plant, and be generated and contained The problem of very high hazardous waste of moisture content not only wastes processing cost, also to pay expensive treatment of sludge expense.
Detailed description of the invention
Fig. 1 is flow diagram of the invention.
Specific embodiment
For the ease of the understanding of those skilled in the art, make below with reference to 1 couple of present invention of examples and drawings further Illustrate, the content that embodiment refers to not is limitation of the invention.
Embodiment 1
A kind of recovery method that phosphate discharge liquid is electroplated, includes the following steps:
1) the first treatment fluid for obtaining the phosphate discharge liquid gathered after oil separator removes the impurity such as organic matter；
2) the first treatment fluid obtained in step 1) is obtained into second processing liquid (raffinate phase) after the first extraction equipment；
3) second processing liquid (raffinate phase) obtained in step 2) is obtained into third treatment fluid after the second extraction equipment (raffinate phase)；
4) third treatment fluid (raffinate phase) obtained in step 3) is obtained into fourth process after the first back extraction device Liquid (raffinate phase)；
5) fourth process liquid (raffinate phase) obtained in step 4) is obtained into the 5th processing after the second back extraction device Liquid (raffinate phase)；
6) the 5th treatment fluid obtained in step 5) is obtained into the 6th treatment fluid after being stripped oil separator；
7) the 6th treatment fluid obtained in step 6) is obtained into the 7th treatment fluid after concentration；
8) final step 7) obtained in the 7th treatment fluid through detect it is up to standard after can be recycled for production line.
First extraction equipment is equipped with No.1 input end, No. two input ends, No.1 outlet end and No. two outlet ends；The Two extraction equipments are equipped with No.1 input end, No. two input ends, No. three input ends, No.1 outlet end and No. two outlet ends；First It is stripped device and is equipped with No.1 input end, No. two input ends, No.1 outlet end and No. two outlet ends；Second back extraction device is set There are No.1 outlet end, No. two outlet ends and No. three outlet ends；The first back extraction oil separator is equipped with No.1 input end and No. two Input end.
Vacuum pressure in the step 7) when concentration is 7.5KPa, and thickening temperature is 70 DEG C；The 7th in step 8) The examination criteria for the treatment of fluid is that water outlet phosphoric acid specific gravity is 1.2, and phosphoric acid concentration is lower than 27.5%, and iron, aluminium content are below 0.1mg/ L。
Extract added with tributyl phosphate in first extraction equipment described in step 2) and step 3) and the second extraction equipment Take agent.
Oil separator described in the step 1) includes the first oil separator and the second oil separator, the outlet of first oil separator End is connected with the input end of second oil separator；First extraction equipment described in step 2) is equipped with No.1 input end, No. two Input end, No.1 outlet end and No. two outlet ends, the No.1 input end of first extraction equipment and second oil separator Outlet end connection；Second extraction equipment described in step 3) is equipped with No.1 input end, No. two input ends, No. three input ends, four Number input end, No.1 outlet end and No. two outlet ends, the No.1 input end of second extraction equipment and first extraction The No.1 outlet end of device is connected to；No. two imports of the No.1 outlet end of second extraction equipment and first extraction equipment End connection；No. four input ends of second extraction equipment are connected to No. two outlet ends of second extraction equipment.
First back extraction device described in step 4) is equipped with No.1 input end, No. two input ends, No.1 outlet end and two The No.1 input end of number outlet end, the first back extraction device is connected to No. two outlet ends of first extraction equipment；Step It is rapid 5) described in second back extraction device be equipped with No.1 outlet end, No. two outlet ends and No. three outlet ends, it is described second back extraction The input end of device is connected to the No.1 outlet end of the first back extraction device；The No.1 outlet of the second back extraction device End is connected to No. two input ends of the second extraction equipment, No. two outlet ends of the second back extraction device and first back extraction No. two input ends of device are taken to be connected to, described second is stripped No. three of No. three outlet ends of device and second extraction equipment Input end connection；Back extraction oil separator described in step 6) includes the first back extraction oil separator and the second back extraction oil separator, institute The first back extraction oil separator is stated equipped with No.1 input end and No. two input ends, No. two outlet ends of the first back extraction device with The No.1 input end connection of the first back extraction oil separator, No. three outlet ends and described first of the second back extraction device It is stripped No. two input ends connection of oil separator, the outlet end of the first back extraction oil separator and the second back extraction oil removal The input end in pond is connected to.
Embodiment 2
A kind of recovery method that phosphate discharge liquid is electroplated, includes the following steps:
1) the first treatment fluid for obtaining the phosphate discharge liquid gathered after oil separator removes the impurity such as organic matter；
2) the first treatment fluid obtained in step 1) is obtained into second processing liquid (raffinate phase) after the first extraction equipment；
3) second processing liquid (raffinate phase) obtained in step 2) is obtained into third treatment fluid after the second extraction equipment (raffinate phase)；
4) third treatment fluid (raffinate phase) obtained in step 3) is obtained into fourth process after the first back extraction device Liquid (raffinate phase)；
5) fourth process liquid (raffinate phase) obtained in step 4) is obtained into the 5th processing after the second back extraction device Liquid (raffinate phase)；
6) the 5th treatment fluid obtained in step 5) is obtained into the 6th treatment fluid after being stripped oil separator；
7) the 6th treatment fluid obtained in step 6) is obtained into the 7th treatment fluid after concentration；
8) final step 7) obtained in the 7th treatment fluid through detect it is up to standard after can be recycled for production line.
First extraction equipment is equipped with No.1 input end, No. two input ends, No.1 outlet end and No. two outlet ends；The Two extraction equipments are equipped with No.1 input end, No. two input ends, No. three input ends, No.1 outlet end and No. two outlet ends；First It is stripped device and is equipped with No.1 input end, No. two input ends, No.1 outlet end and No. two outlet ends；Second back extraction device is set There are No.1 outlet end, No. two outlet ends and No. three outlet ends；The first back extraction oil separator is equipped with No.1 input end and No. two Input end.
Vacuum pressure in the step 7) when concentration is 7.75KPa, and thickening temperature is 73 DEG C；The 7th in step 8) The examination criteria for the treatment of fluid is that water outlet phosphoric acid specific gravity is 1.22, and phosphoric acid concentration is lower than 27.5%, and iron, aluminium content are below 0.1mg/ L。
Extract added with tributyl phosphate in first extraction equipment described in step 2) and step 3) and the second extraction equipment Take agent.
Oil separator described in the step 1) includes the first oil separator and the second oil separator, the outlet of first oil separator End is connected with the input end of second oil separator；First extraction equipment described in step 2) is equipped with No.1 input end, No. two Input end, No.1 outlet end and No. two outlet ends, the No.1 input end of first extraction equipment and second oil separator Outlet end connection；Second extraction equipment described in step 3) is equipped with No.1 input end, No. two input ends, No. three input ends, four Number input end, No.1 outlet end and No. two outlet ends, the No.1 input end of second extraction equipment and first extraction The No.1 outlet end of device is connected to；No. two imports of the No.1 outlet end of second extraction equipment and first extraction equipment End connection；No. four input ends of second extraction equipment are connected to No. two outlet ends of second extraction equipment.
First back extraction device described in step 4) is equipped with No.1 input end, No. two input ends, No.1 outlet end and two The No.1 input end of number outlet end, the first back extraction device is connected to No. two outlet ends of first extraction equipment；Step It is rapid 5) described in second back extraction device be equipped with No.1 outlet end, No. two outlet ends and No. three outlet ends, it is described second back extraction The input end of device is connected to the No.1 outlet end of the first back extraction device；The No.1 outlet of the second back extraction device End is connected to No. two input ends of the second extraction equipment, No. two outlet ends of the second back extraction device and first back extraction No. two input ends of device are taken to be connected to, described second is stripped No. three of No. three outlet ends of device and second extraction equipment Input end connection；Back extraction oil separator described in step 6) includes the first back extraction oil separator and the second back extraction oil separator, institute The first back extraction oil separator is stated equipped with No.1 input end and No. two input ends, No. two outlet ends of the first back extraction device with The No.1 input end connection of the first back extraction oil separator, No. three outlet ends and described first of the second back extraction device It is stripped No. two input ends connection of oil separator, the outlet end of the first back extraction oil separator and the second back extraction oil removal The input end in pond is connected to.
Embodiment 3
A kind of recovery method that phosphate discharge liquid is electroplated, includes the following steps:
1) the first treatment fluid for obtaining the phosphate discharge liquid gathered after oil separator removes the impurity such as organic matter；
2) the first treatment fluid obtained in step 1) is obtained into second processing liquid (raffinate phase) after the first extraction equipment；
3) second processing liquid (raffinate phase) obtained in step 2) is obtained into third treatment fluid after the second extraction equipment (raffinate phase)；
4) third treatment fluid (raffinate phase) obtained in step 3) is obtained into fourth process after the first back extraction device Liquid (raffinate phase)；
5) fourth process liquid (raffinate phase) obtained in step 4) is obtained into the 5th processing after the second back extraction device Liquid (raffinate phase)；
6) the 5th treatment fluid obtained in step 5) is obtained into the 6th treatment fluid after being stripped oil separator；
7) the 6th treatment fluid obtained in step 6) is obtained into the 7th treatment fluid after concentration；
8) final step 7) obtained in the 7th treatment fluid through detect it is up to standard after can be recycled for production line.
First extraction equipment is equipped with No.1 input end, No. two input ends, No.1 outlet end and No. two outlet ends；The Two extraction equipments are equipped with No.1 input end, No. two input ends, No. three input ends, No.1 outlet end and No. two outlet ends；First It is stripped device and is equipped with No.1 input end, No. two input ends, No.1 outlet end and No. two outlet ends；Second back extraction device is set There are No.1 outlet end, No. two outlet ends and No. three outlet ends；The first back extraction oil separator is equipped with No.1 input end and No. two Input end.
Vacuum pressure in the step 7) when concentration is 8KPa, and thickening temperature is 75 DEG C；At the 7th in step 8) The examination criteria of reason liquid is that water outlet phosphoric acid specific gravity is 1.24, and phosphoric acid concentration is lower than 27.5%, and iron, aluminium content are below 0.1mg/L.
Extract added with tributyl phosphate in first extraction equipment described in step 2) and step 3) and the second extraction equipment Take agent.
Oil separator described in the step 1) includes the first oil separator and the second oil separator, the outlet of first oil separator End is connected with the input end of second oil separator；First extraction equipment described in step 2) is equipped with No.1 input end, No. two Input end, No.1 outlet end and No. two outlet ends, the No.1 input end of first extraction equipment and second oil separator Outlet end connection；Second extraction equipment described in step 3) is equipped with No.1 input end, No. two input ends, No. three input ends, four Number input end, No.1 outlet end and No. two outlet ends, the No.1 input end of second extraction equipment and first extraction The No.1 outlet end of device is connected to；No. two imports of the No.1 outlet end of second extraction equipment and first extraction equipment End connection；No. four input ends of second extraction equipment are connected to No. two outlet ends of second extraction equipment.
First back extraction device described in step 4) is equipped with No.1 input end, No. two input ends, No.1 outlet end and two The No.1 input end of number outlet end, the first back extraction device is connected to No. two outlet ends of first extraction equipment；Step It is rapid 5) described in second back extraction device be equipped with No.1 outlet end, No. two outlet ends and No. three outlet ends, it is described second back extraction The input end of device is connected to the No.1 outlet end of the first back extraction device；The No.1 outlet of the second back extraction device End is connected to No. two input ends of the second extraction equipment, No. two outlet ends of the second back extraction device and first back extraction No. two input ends of device are taken to be connected to, described second is stripped No. three of No. three outlet ends of device and second extraction equipment Input end connection；Back extraction oil separator described in step 6) includes the first back extraction oil separator and the second back extraction oil separator, institute The first back extraction oil separator is stated equipped with No.1 input end and No. two input ends, No. two outlet ends of the first back extraction device with The No.1 input end connection of the first back extraction oil separator, No. three outlet ends and described first of the second back extraction device It is stripped No. two input ends connection of oil separator, the outlet end of the first back extraction oil separator and the second back extraction oil removal The input end in pond is connected to.
Embodiment 4
A kind of recovery method that phosphate discharge liquid is electroplated, includes the following steps:
1) the first treatment fluid for obtaining the phosphate discharge liquid gathered after oil separator removes the impurity such as organic matter；
2) the first treatment fluid obtained in step 1) is obtained into second processing liquid (raffinate phase) after the first extraction equipment；
3) second processing liquid (raffinate phase) obtained in step 2) is obtained into third treatment fluid after the second extraction equipment (raffinate phase)；
4) third treatment fluid (raffinate phase) obtained in step 3) is obtained into fourth process after the first back extraction device Liquid (raffinate phase)；
5) fourth process liquid (raffinate phase) obtained in step 4) is obtained into the 5th processing after the second back extraction device Liquid (raffinate phase)；
6) the 5th treatment fluid obtained in step 5) is obtained into the 6th treatment fluid after being stripped oil separator；
7) the 6th treatment fluid obtained in step 6) is obtained into the 7th treatment fluid after concentration；
8) final step 7) obtained in the 7th treatment fluid through detect it is up to standard after can be recycled for production line.
First extraction equipment is equipped with No.1 input end, No. two input ends, No.1 outlet end and No. two outlet ends；The Two extraction equipments are equipped with No.1 input end, No. two input ends, No. three input ends, No.1 outlet end and No. two outlet ends；First It is stripped device and is equipped with No.1 input end, No. two input ends, No.1 outlet end and No. two outlet ends；Second back extraction device is set There are No.1 outlet end, No. two outlet ends and No. three outlet ends；The first back extraction oil separator is equipped with No.1 input end and No. two Input end.
Vacuum pressure in the step 7) when concentration is 8.25KPa, and thickening temperature is 78 DEG C；The 7th in step 8) The examination criteria for the treatment of fluid is that water outlet phosphoric acid specific gravity is 1.26, and phosphoric acid concentration is lower than 27.5%, and iron, aluminium content are below 0.1mg/ L。
Extract added with tributyl phosphate in first extraction equipment described in step 2) and step 3) and the second extraction equipment Take agent.
Oil separator described in the step 1) includes the first oil separator and the second oil separator, the outlet of first oil separator End is connected with the input end of second oil separator；First extraction equipment described in step 2) is equipped with No.1 input end, No. two Input end, No.1 outlet end and No. two outlet ends, the No.1 input end of first extraction equipment and second oil separator Outlet end connection；Second extraction equipment described in step 3) is equipped with No.1 input end, No. two input ends, No. three input ends, four Number input end, No.1 outlet end and No. two outlet ends, the No.1 input end of second extraction equipment and first extraction The No.1 outlet end of device is connected to；No. two imports of the No.1 outlet end of second extraction equipment and first extraction equipment End connection；No. four input ends of second extraction equipment are connected to No. two outlet ends of second extraction equipment.
First back extraction device described in step 4) is equipped with No.1 input end, No. two input ends, No.1 outlet end and two The No.1 input end of number outlet end, the first back extraction device is connected to No. two outlet ends of first extraction equipment；Step It is rapid 5) described in second back extraction device be equipped with No.1 outlet end, No. two outlet ends and No. three outlet ends, it is described second back extraction The input end of device is connected to the No.1 outlet end of the first back extraction device；The No.1 outlet of the second back extraction device End is connected to No. two input ends of the second extraction equipment, No. two outlet ends of the second back extraction device and first back extraction No. two input ends of device are taken to be connected to, described second is stripped No. three of No. three outlet ends of device and second extraction equipment Input end connection；Back extraction oil separator described in step 6) includes the first back extraction oil separator and the second back extraction oil separator, institute The first back extraction oil separator is stated equipped with No.1 input end and No. two input ends, No. two outlet ends of the first back extraction device with The No.1 input end connection of the first back extraction oil separator, No. three outlet ends and described first of the second back extraction device It is stripped No. two input ends connection of oil separator, the outlet end of the first back extraction oil separator and the second back extraction oil removal The input end in pond is connected to.
Embodiment 5
A kind of recovery method that phosphate discharge liquid is electroplated, includes the following steps:
1) the first treatment fluid for obtaining the phosphate discharge liquid gathered after oil separator removes the impurity such as organic matter；
2) the first treatment fluid obtained in step 1) is obtained into second processing liquid (raffinate phase) after the first extraction equipment；
3) second processing liquid (raffinate phase) obtained in step 2) is obtained into third treatment fluid after the second extraction equipment (raffinate phase)；
4) third treatment fluid (raffinate phase) obtained in step 3) is obtained into fourth process after the first back extraction device Liquid (raffinate phase)；
5) fourth process liquid (raffinate phase) obtained in step 4) is obtained into the 5th processing after the second back extraction device Liquid (raffinate phase)；
6) the 5th treatment fluid obtained in step 5) is obtained into the 6th treatment fluid after being stripped oil separator；
7) the 6th treatment fluid obtained in step 6) is obtained into the 7th treatment fluid after concentration；
8) final step 7) obtained in the 7th treatment fluid through detect it is up to standard after can be recycled for production line.
First extraction equipment is equipped with No.1 input end, No. two input ends, No.1 outlet end and No. two outlet ends；The Two extraction equipments are equipped with No.1 input end, No. two input ends, No. three input ends, No.1 outlet end and No. two outlet ends；First It is stripped device and is equipped with No.1 input end, No. two input ends, No.1 outlet end and No. two outlet ends；Second back extraction device is set There are No.1 outlet end, No. two outlet ends and No. three outlet ends；The first back extraction oil separator is equipped with No.1 input end and No. two Input end.
Vacuum pressure in the step 7) when concentration is 8.5KPa, and thickening temperature is 80 DEG C；The 7th in step 8) The examination criteria for the treatment of fluid is that water outlet phosphoric acid specific gravity is 1.3, and phosphoric acid concentration is lower than 27.5%, and iron, aluminium content are below 0.1mg/ L。
Extract added with tributyl phosphate in first extraction equipment described in step 2) and step 3) and the second extraction equipment Take agent.
Oil separator described in the step 1) includes the first oil separator and the second oil separator, the outlet of first oil separator End is connected with the input end of second oil separator；First extraction equipment described in step 2) is equipped with No.1 input end, No. two Input end, No.1 outlet end and No. two outlet ends, the No.1 input end of first extraction equipment and second oil separator Outlet end connection；Second extraction equipment described in step 3) is equipped with No.1 input end, No. two input ends, No. three input ends, four Number input end, No.1 outlet end and No. two outlet ends, the No.1 input end of second extraction equipment and first extraction The No.1 outlet end of device is connected to；No. two imports of the No.1 outlet end of second extraction equipment and first extraction equipment End connection；No. four input ends of second extraction equipment are connected to No. two outlet ends of second extraction equipment.
First back extraction device described in step 4) is equipped with No.1 input end, No. two input ends, No.1 outlet end and two The No.1 input end of number outlet end, the first back extraction device is connected to No. two outlet ends of first extraction equipment；Step It is rapid 5) described in second back extraction device be equipped with No.1 outlet end, No. two outlet ends and No. three outlet ends, it is described second back extraction The input end of device is connected to the No.1 outlet end of the first back extraction device；The No.1 outlet of the second back extraction device End is connected to No. two input ends of the second extraction equipment, No. two outlet ends of the second back extraction device and first back extraction No. two input ends of device are taken to be connected to, described second is stripped No. three of No. three outlet ends of device and second extraction equipment Input end connection；Back extraction oil separator described in step 6) includes the first back extraction oil separator and the second back extraction oil separator, institute The first back extraction oil separator is stated equipped with No.1 input end and No. two input ends, No. two outlet ends of the first back extraction device with The No.1 input end connection of the first back extraction oil separator, No. three outlet ends and described first of the second back extraction device It is stripped No. two input ends connection of oil separator, the outlet end of the first back extraction oil separator and the second back extraction oil removal The input end in pond is connected to.
Comparative example 1
A kind of recovery method that phosphate discharge liquid is electroplated, includes the following steps:
1) the first treatment fluid for obtaining the phosphate discharge liquid gathered after oil separator removes the impurity such as organic matter；
2) the first treatment fluid obtained in step 1) is obtained into second processing liquid (raffinate phase) after the first extraction equipment；
3) second processing liquid (raffinate phase) obtained in step 2) is obtained into third treatment fluid after the second extraction equipment (raffinate phase)；
4) third treatment fluid (raffinate phase) obtained in step 3) is obtained into fourth process after the first back extraction device Liquid (raffinate phase)；
5) fourth process liquid (raffinate phase) obtained in step 4) is obtained into the 5th processing after the second back extraction device Liquid (raffinate phase)；
6) the 5th treatment fluid obtained in step 5) is obtained into the 6th treatment fluid after being stripped oil separator；
7) the 6th treatment fluid obtained in step 6) is obtained into the 7th treatment fluid after concentration；
8) final step 7) obtained in the 7th treatment fluid through detect it is up to standard after can be recycled for production line.
First extraction equipment is equipped with No.1 input end, No. two input ends, No.1 outlet end and No. two outlet ends；The Two extraction equipments are equipped with No.1 input end, No. two input ends, No. three input ends, No.1 outlet end and No. two outlet ends；First It is stripped device and is equipped with No.1 input end, No. two input ends, No.1 outlet end and No. two outlet ends；Second back extraction device is set There are No.1 outlet end, No. two outlet ends and No. three outlet ends；The first back extraction oil separator is equipped with No.1 input end and No. two Input end.
Vacuum pressure in the step 7) when concentration is 7.5KPa, and thickening temperature is 70 DEG C；The 7th in step 8) The examination criteria for the treatment of fluid is that water outlet phosphoric acid specific gravity is 1.2, and phosphoric acid concentration is lower than 27.5%, and iron, aluminium content are below 0.1mg/ L。
Extract added with tributyl phosphate in first extraction equipment described in step 2) and step 3) and the second extraction equipment Take agent.
The No.1 input end of first extraction equipment described in step 2) is connected to the outlet end of the oil separator；In step 3) The No.1 input end of second extraction equipment is connected to the No.1 outlet end of first extraction equipment；The second extraction dress The outlet end set is connected to No. two input ends of first extraction equipment.
No. two outlet ends of the No.1 input end of the first back extraction device and first extraction equipment described in step 4) Connection；Second back extraction device described in step 5) is equipped with No.1 outlet end and No. two outlet ends, the second back extraction device Input end with it is described first back extraction device No.1 outlet end be connected to；It is described second back extraction device No.1 outlet end with No. two input ends connection of the first back extraction device；Back extraction oil separator described in step 6) includes the first back extraction oil removal Pond and second back extraction oil separator, it is described first back extraction oil separator be equipped with No.1 input end and No. two input ends, described first No. two outlet ends for being stripped device are connected to the No.1 input end of the first back extraction oil separator, the second back extraction dress No. two outlet ends set are connected to No. two input ends of the first back extraction oil separator, and the first back extraction oil separator goes out Mouth end is connected to the input end of the second back extraction oil separator.
Comparative example 2
A kind of recovery method that phosphate discharge liquid is electroplated, includes the following steps:
1) the first treatment fluid for obtaining the phosphate discharge liquid gathered after oil separator removes the impurity such as organic matter；
2) the first treatment fluid obtained in step 1) is obtained into second processing liquid (raffinate phase) after the first extraction equipment；
3) second processing liquid (raffinate phase) obtained in step 2) is obtained into third processing after the first back extraction device Liquid (raffinate phase)；
4) third treatment fluid (raffinate phase) obtained in step 3) is obtained into fourth process after the second back extraction device Liquid (raffinate phase)；
5) fourth process liquid (raffinate phase) obtained in step 4) is obtained into the 5th treatment fluid after being stripped oil separator；
6) the 5th treatment fluid obtained in step 5) is obtained into the 6th treatment fluid after concentration；
7) final step 6) obtained in the 6th treatment fluid through detect it is up to standard after can be recycled for production line.
First extraction equipment is equipped with No.1 input end, No. two input ends and No.1 outlet end；First back extraction Device is taken to be equipped with No.1 input end, No. two input ends, No.1 outlet end and No. two outlet ends；The second back extraction device is set There are No.1 outlet end and No. two outlet ends.
Vacuum pressure in the step 7) when concentration is 8KPa, and thickening temperature is 75 DEG C；At the 7th in step 8) The examination criteria of reason liquid is that water outlet phosphoric acid specific gravity is 1.26, and phosphoric acid concentration is lower than 27.5%, and iron, aluminium content are below 0.1mg/L.
Calcium phosphate+ forage agent is added in first extraction equipment described in step 2).
Oil separator described in the step 1) includes the first oil separator and the second oil separator, the outlet of first oil separator End is connected with the input end of second oil separator；The No.1 input end of first extraction equipment described in step 2) and described the The outlet end of two oil separators is connected to.
No. two outlet ends of the No.1 input end of the first back extraction device and first extraction equipment described in step 4) Connection；The input end of second back extraction device described in step 5) is connected to the No.1 outlet end of the first back extraction device； The outlet end of the second back extraction device is connected to No. two input ends of the first extraction equipment；Described in step 6) back extraction every Oil sump includes the first back extraction oil separator and the second back extraction oil separator, and described first is stripped No. two outlet ends of device and institute State the first back extraction oil separator input end connection, it is described first back extraction oil separator outlet end and it is described second back extraction every The input end of oil sump is connected to.
Comparative example 3
A kind of recovery method that phosphate discharge liquid is electroplated, includes the following steps:
1) the first treatment fluid for obtaining the phosphate discharge liquid gathered after oil separator removes the impurity such as organic matter；
2) the first treatment fluid obtained in step 1) is obtained into second processing liquid after the first extraction equipment；
3) second processing liquid obtained in step 2) is obtained into third treatment fluid after the second extraction equipment；
4) third treatment fluid obtained in step 3) is obtained into fourth process liquid after the first back extraction device；
5) fourth process liquid obtained in step 4) is obtained into the 5th treatment fluid after the second back extraction device；
6) the 5th treatment fluid obtained in step 5) is obtained into the 6th treatment fluid after being stripped oil separator；
7) the 6th treatment fluid obtained in step 6) is obtained into the 7th treatment fluid after concentration；
8) final step 7) obtained in the 7th treatment fluid through detect it is up to standard after can be recycled for production line.
First extraction equipment is equipped with No.1 input end, No. two input ends, No.1 outlet end and No. two outlet ends；The Two extraction equipments are equipped with No.1 input end, No. two input ends, No. three input ends, No.1 outlet end and No. two outlet ends；First It is stripped device and is equipped with No.1 input end, No. two input ends, No.1 outlet end and No. two outlet ends；Second back extraction device is set There are No.1 outlet end, No. two outlet ends and No. three outlet ends；The first back extraction oil separator is equipped with No.1 input end and No. two Input end.
Vacuum pressure in the step 7) when concentration is 8.5KPa, and thickening temperature is 80 DEG C；The 7th in step 8) The examination criteria for the treatment of fluid is that water outlet phosphoric acid specific gravity is 1.3, and phosphoric acid concentration is lower than 27.5%, and iron, aluminium content are below 0.1mg/ L。
Oil separator described in the step 1) includes the first oil separator and the second oil separator, the outlet of first oil separator End is connected with the input end of second oil separator；First extraction equipment described in step 2) is equipped with No.1 input end, No. two Input end, No.1 outlet end and No. two outlet ends, the No.1 input end of first extraction equipment and second oil separator Outlet end connection；Second extraction equipment described in step 3) is equipped with No.1 input end, No. two input ends, No. three input ends, four Number input end, No.1 outlet end and No. two outlet ends, the No.1 input end of second extraction equipment and first extraction The No.1 outlet end of device is connected to；No. two imports of the No.1 outlet end of second extraction equipment and first extraction equipment End connection；No. four input ends of second extraction equipment are connected to No. two outlet ends of second extraction equipment.
First back extraction device described in step 4) is equipped with No.1 input end, No. two input ends, No.1 outlet end and two The No.1 input end of number outlet end, the first back extraction device is connected to No. two outlet ends of first extraction equipment；Step It is rapid 5) described in second back extraction device be equipped with No.1 outlet end, No. two outlet ends and No. three outlet ends, it is described second back extraction The input end of device is connected to the No.1 outlet end of the first back extraction device；The No.1 outlet of the second back extraction device End is connected to No. two input ends of the second extraction equipment, No. two outlet ends of the second back extraction device and first back extraction No. two input ends of device are taken to be connected to, described second is stripped No. three of No. three outlet ends of device and second extraction equipment Input end connection；Back extraction oil separator described in step 6) includes the first back extraction oil separator and the second back extraction oil separator, institute The first back extraction oil separator is stated equipped with No.1 input end and No. two input ends, No. two outlet ends of the first back extraction device with The No.1 input end connection of the first back extraction oil separator, No. three outlet ends and described first of the second back extraction device It is stripped No. two input ends connection of oil separator, the outlet end of the first back extraction oil separator and the second back extraction oil removal The input end in pond is connected to.
It respectively will treated that standard is given up containing specific embodiment 1-5 treated normal wastewater and containing comparative example 1-3 It is as shown in table 1 below that water carries out iron, aluminium content measurement result:
Table 1
From the above results, iron, aluminium content are below in the recovered liquid after processing in 1-5 of the embodiment of the present invention 0.1mg/L, and method processing sewage of the invention is high-efficient, not only reduces processing cost, and after processing recycling Phosphoric acid can also be back on production line, a large amount of Dephosphorization reagent will be consumed by avoiding conventional treatment and being discharged to sewage plant.
Compared with Example 1, comparative example 1 only passes through an oil separator in phosphate discharge liquid processing, to utilization 1 institute of comparative example Recovered liquid after stating process carries out iron, aluminium content test and organic matter test, it is found that its iron, aluminium content are promoted, Content of organics is apparently higher than in embodiment 1 and handles recovered liquid；Illustrate that the present invention can by the processing of two oil separators in phosphate discharge liquid To reduce the impurity such as iron, aluminium, organic matter well.
Compared with Example 3, comparative example 2 only passes through single extraction in phosphate discharge liquid processing, to using described in comparative example 2 Recovered liquid after process carries out iron, aluminium content test and organic matter test, it is found that its iron, aluminium content are obviously improved；It says The bright present invention can reduce the impurity such as iron, aluminium, organic matter by the processing of abstraction pool twice in phosphate discharge liquid well.
Compared with Example 5, the reextraction in phosphate discharge liquid processing of comparative example 3 does not add calcium phosphate+ forage Agent is tested iron, aluminium content test and organic matter is carried out using the recovered liquid after process described in comparative example 3, finds it Iron, aluminium content survey are promoted；Illustrate that the present invention has addition calcium phosphate+ forage agent processing in phosphate discharge liquid reextraction The impurity such as organic matter can be removed well.
Above-described embodiment is the preferable implementation of the present invention, and in addition to this, the present invention can be realized with other way, Do not depart under the premise of present inventive concept it is any obviously replace it is within the scope of the present invention.

Claims (10)

1. a kind of recovery method that phosphate discharge liquid is electroplated, characterized by the following steps:
1) the first treatment fluid for obtaining the phosphate discharge liquid gathered after oil separator removes impurity；
2) the first treatment fluid obtained in step 1) is obtained into second processing liquid after the processing of the first extraction equipment；
3) second processing liquid obtained in step 2) is obtained into third treatment fluid after the processing of the second extraction equipment；
4) third treatment fluid obtained in step 3) is obtained into fourth process liquid after the first back extraction device processing；
5) fourth process liquid obtained in step 4) is obtained into the 5th treatment fluid after the second back extraction device processing；
6) the 5th treatment fluid obtained in step 5) is obtained into the 6th treatment fluid after back extraction oil separator processing；
7) the 6th treatment fluid obtained in step 6) is obtained into the 7th treatment fluid after concentration；
8) the 7th treatment fluid obtained in step 7) can be recycled after detection is up to standard for production line.
2. a kind of recovery method that phosphate discharge liquid is electroplated according to claim 1, it is characterised in that: the step 7) concentration Vacuum pressure when processing is 7.5-8.5KPa, and thickening temperature is 70-80 DEG C.
3. a kind of recovery method that phosphate discharge liquid is electroplated according to claim 1, it is characterised in that: the described in step 2) Calcium phosphate+ forage agent is added in second extraction equipment described in one extraction equipment and step 3).
4. a kind of recovery method that phosphate discharge liquid is electroplated according to claim 1, it is characterised in that: institute in the step 1) Stating oil separator includes the first oil separator and the second oil separator, the outlet end of first oil separator and second oil separator into Mouth end is connected.
5. a kind of recovery method that phosphate discharge liquid is electroplated according to claim 4, it is characterised in that: the described in step 2) One extraction equipment is equipped with No.1 input end, No. two input ends, No.1 outlet end and No. two outlet ends, first extraction equipment No.1 input end be connected to the outlet end of second oil separator.
6. a kind of recovery method that phosphate discharge liquid is electroplated according to claim 5, it is characterised in that: the described in step 3) Two extraction equipments are equipped with No.1 input end, No. two input ends, No. three input ends, No. four input ends, No.1 outlet end and No. two Outlet end, the No.1 input end of second extraction equipment are connected to the No.1 outlet end of first extraction equipment；Described The No.1 outlet end of two extraction equipments is connected to No. two input ends of first extraction equipment；The four of second extraction equipment Number input end is connected to No. two outlet ends of second extraction equipment.
7. a kind of recovery method that phosphate discharge liquid is electroplated according to claim 5, it is characterised in that: the described in step 4) One back extraction device is equipped with No.1 input end, No. two input ends, No.1 outlet end and No. two outlet ends, first back extraction The No.1 input end of device is connected to No. two outlet ends of first extraction equipment.
8. a kind of recovery method that phosphate discharge liquid is electroplated according to claim 6, it is characterised in that: the described in step 5) Two back extraction devices are equipped with No.1 outlet end, No. two outlet ends and No. three outlet ends, the input end of the second back extraction device It is connected to the No.1 outlet end of the first back extraction device；The No.1 outlet end of the second back extraction device and the second extraction No. two input ends of device are connected to, No. two outlet ends and the described first No. two for being stripped device of the second back extraction device No. three outlet ends of input end connection, the second back extraction device are connected to No. three input ends of second extraction equipment.
9. a kind of recovery method that phosphate discharge liquid is electroplated according to claim 1, it is characterised in that: the described in step 4) One back extraction device is equipped with No.1 input end, No. two input ends, No.1 outlet end and No. two outlet ends；Described in step 5) Two back extraction devices are equipped with No.1 outlet end and No. two outlet ends；Back extraction oil separator described in step 6) includes the first back extraction Oil separator and the second back extraction oil separator, the first back extraction oil separator is equipped with No.1 input end and No. two input ends, described No. two outlet ends of the first back extraction device are connected to the No.1 input end of the first back extraction oil separator, second back extraction No. three outlet ends of device and No. two input ends of the first back extraction oil separator are taken to be connected to, the first back extraction oil separator Outlet end with it is described second back extraction oil separator input end be connected to.
10. a kind of recovery method that phosphate discharge liquid is electroplated according to claim 1, it is characterised in that: the 7th in step 8) The examination criteria for the treatment of fluid is that water outlet phosphoric acid specific gravity is 1.2-1.3, and phosphoric acid concentration is lower than 27.5%, and iron, aluminium content are below 0.1mg/L。
CN201910266579.9A 2019-04-03 2019-04-03 A kind of recovery method that phosphate discharge liquid is electroplated Pending CN110040864A (en)

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