CN109502833A - A kind of use in waste water treatment flocculant and preparation method thereof - Google Patents

A kind of use in waste water treatment flocculant and preparation method thereof Download PDF

Info

Publication number
CN109502833A
CN109502833A CN201910009241.5A CN201910009241A CN109502833A CN 109502833 A CN109502833 A CN 109502833A CN 201910009241 A CN201910009241 A CN 201910009241A CN 109502833 A CN109502833 A CN 109502833A
Authority
CN
China
Prior art keywords
parts
preparation
phosphorous
waste water
flocculant
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201910009241.5A
Other languages
Chinese (zh)
Inventor
毛强平
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN201910009241.5A priority Critical patent/CN109502833A/en
Publication of CN109502833A publication Critical patent/CN109502833A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00Multistage treatment of water, waste water or sewage
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/001Processes for the treatment of water whereby the filtration technique is of importance
    • 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
    • C02F1/34Treatment of water, waste water, or sewage with mechanical oscillations
    • C02F1/36Treatment of water, waste water, or sewage with mechanical oscillations ultrasonic vibrations
    • 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
    • C02F1/44Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
    • C02F1/441Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
    • 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
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • 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
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • C02F1/5245Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
    • 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
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/54Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
    • C02F1/56Macromolecular compounds
    • 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
    • C02F1/66Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • 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
    • C02F1/72Treatment of water, waste water, or sewage by oxidation
    • 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
    • C02F1/72Treatment of water, waste water, or sewage by oxidation
    • C02F1/727Treatment of water, waste water, or sewage by oxidation using pure oxygen or oxygen rich gas
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/105Phosphorus compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00Controlling or monitoring parameters in water treatment
    • C02F2209/08Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00Controlling or monitoring parameters in water treatment
    • C02F2209/22O2
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2301/00General aspects of water treatment
    • C02F2301/08Multistage treatments, e.g. repetition of the same process step under different conditions

Abstract

The present invention provides a kind of flocculants applied to wastewater treatment to belong to technical field of water treatment chemical more particularly to the flocculant for the processing for being applied to phosphorous oily waste water.The flocculant that the present invention uses is a kind of flocculant of modified polyacrylamide, has the effect of preferably removing COD, sediment and oils for phosphorous oiliness sewage treatment.

Description

A kind of use in waste water treatment flocculant and preparation method thereof
Technical field
The present invention be number of patent application be 2016106042384, the applying date is on 07 28th, 2016, entitled " a kind of The processing method of phosphorous oily waste water " patent of invention divisional application.
The present invention provides a kind of flocculants applied to wastewater treatment, more particularly to applied to phosphorous oily waste water The flocculant of processing, belongs to technical field of water treatment chemical.
Background technique
Certain mechanical technologies will largely be made using the emulsion of oil-in-water type especially in the machinings such as cutting, grinding Lubrication, cooling circulation liquid.Its main ingredient is machine oil or dormant oil (can also use animal and vegetable oil), emulsifier, lubricating and antirust agent and water Emulsifier often uses sulfonated oil, petroleum sodium sulfonate and oleic acid etc..Antirust agent often uses zinc naphthenate, barium mahogany sulfonate, sodium nitrite, three Ethanol amine, certain benzene homologues etc..In emulsion, although the content of oil emulsion is not high, less than 1% in emulsifying waste water.But It is, due to the surface-active action of emulsifier, so that the structure of emulsion is highly stable, to be not easy to be destroyed.In certain emulsions Mineral oil and additive toxicity it is very big, contain carcinogen.Such a waste emulsified mixture, if do not dealt with, direct emission, On the pollution of environment and influence, than general oily wastewater zhang much.Therefore, to mechanical oily waste water, wherein especially elbow The processing and prevention and treatment of emulsifying waste water, are very necessary.
In addition, the waste water discharged in machining industry can also be brought more serious other than bringing serious oily pollution Phosphorus pollution.These pollution hands will be from machine plus the phosphorization treatment process in industry.So-called phosphorating treatment be to metal material and A kind of chemical reprocessing technique that its article surface carries out.Dipped type is formed through parkerized metal material and its product surface Phosphate film layer, the film layer and metallic matrix have good binding ability, wearability and the adhesive ability to coating, therefore, machine The industries such as tool, steel all use phosphorization treatment technology to carry out the protective layer of production machinery part.Phosphorization treatment process generally comprises alkali Remove several steps such as oil, hot water rinsing, cold rinse, acid pickling and rust removing, secondary cold rinse and phosphatization.It is main during its Generate four kinds of waste water such as alkali-wash waste water, poaching wastewater, pickle liquor and etching waste liquor.
The elements such as phosphorus, nitrogen are exceeded in water, can accelerate the eutrophication of water body, and this phenomenon is more serious in China, give work Industry, aquatic products industry, agricultural and tourist industry all bring great harm.The nutrient concentrations such as nitrogen, phosphorus increase, and are that algae is a large amount of The reason of breeding, wherein again using phosphorus as key factor.Therefore, the concentration of phosphor in sewage how is effectively reduced, offsets depollution, protects Retaining ring border, has a very important significance.Currently, sewage dephosphorization technology mainly has bioanalysis, chemical method two major classes both at home and abroad.It is raw Object method such as A/O, A2/O technique are mainly suitable for processing low concentration and organic phosphorus-containing wastewater;Chemical method and physical-chemical process are main There are the techniques such as coagulant sedimentation, crystallisation, ion exchange adsorption, electrodialysis, reverse osmosis, it is phosphorous to be mainly suitable for processing inorganic states Waste water.
CN105417785A discloses a kind of reaction unit for handling high-concentration phosphorus-containing wastewater, is pre-processed by desulfurization wastewater single Member, phosphorus recovery unit, deep phosphorous removal unit and desulfurization wastewater sludge pump form, and are provided with desulfurization in desulfurization wastewater pretreatment unit Water intake, dosing mouth, blender, desulfurization wastewater supernatant water outlet and desulfurization wastewater mud discharging mouth;Phosphorus recovery unit In be provided with high-concentration phosphorus-containing wastewater water inlet, blender, phosphorus-containing wastewater water outlet and phosphorous sediment discharge mouth;Deep phosphorous removal The import of desulfurization wastewater sludge, blender, total water outlet and mud discharging mouth are provided in unit.Desulfurization wastewater after pretreatment can Heavy metal and suspended matter therein are enough removed, the supernatant of high ph-values, high calcium magnesium ion is formed, is formed with high-concentration phosphorus-containing wastewater The very low phosphorous sediment of height of content of beary metal;Phosphorus-containing wastewater after dephosphorization enters deep phosphorous removal unit, utilizes desulfurization wastewater dirt Mud carries out chemisorption dephosphorization to phosphorus-containing wastewater, reduces water outlet phosphorus concentration, reaches discharge standard.CN103159341A discloses one Kind treatment of Phosphorus Containing Waste Water technique.The treatment process includes the following steps: phosphorus-containing wastewater and oxidant after mixing, through pH tune It saves agent adjustment pH value and obtains positive phosphorus acid ion to 4~6 progress oxidation reactions, then pH value is adjusted to 7~9 with pH adjusting agent to make just Metal ion contained in phosphate radical and oxidant, which generates, to be precipitated, and precipitating is removed.
But above-mentioned method is bad for oil-containing and phosphorous water treatment effect simultaneously.
Summary of the invention
The purpose of the present invention is: solve the problems, such as the processing of the waste water simultaneously containing high concentration phosphorus and grease type COD, mainly It is handled by the integration mode of oxidation, precipitating, ultrasonic wave added.
Technical solution is:
A kind of processing method of phosphorous oily waste water, includes the following steps:
Phosphorous oily waste water is first carried out pre-filtering, then is handled by wet oxidation by step 1;
The pH of feed liquid after oxidation processes is adjusted to 9~11 by step 2, then under conditions of ultrasonic wave added, and calcium precipitation is added Agent and polyacrylamide flocculant carry out precipitation reaction and obtain the first feed liquid after removal precipitates;
The pH of first feed liquid is adjusted to 3~5, aluminium polychloride is added by step 3, carries out flocculation precipitation reaction, removal precipitating Afterwards, the second feed liquid is obtained;
Second feed liquid is sent into reverse osmosis membrane and be filtered, obtains that treated and produce water by step 4.
Contain 0.1~5g/L of mineral oil, 0.1~3g/L of total phosphorus (TP) concentration in the phosphorous oily waste water.
The mineral oil is white oil, and the total phosphorus is made of phosphate, hypophosphites, phosphite.
In the step 1, the temperature range of wet oxidation is 125~220 DEG C, pressure limit is 0.5~5Mpa, oxygen 1~4g/L of gas additional amount.
In the step 1, ultrasound condition is 400~600kHz of frequency, 1~5W/cm of ultrasonic power2
The calcium precipitation agent is selected from that calcium chloride, calcium oxide are one or more, the additional amount of calcium precipitation agent and total phosphorus Molar ratio range is 2~4:1.
The additional amount of polyacrylamide is 0.5~3g/L.
The additional amount of aluminium polychloride is 1~5g/L respectively.
The preparation method of the polyacrylamide flocculant includes the following steps: S1, by weight, in reactor Middle 35 parts of addition acrylamide monomer, 2 parts of tung oil, 3 parts of 2- acrylamido -2- methyl propane sulfonic acid (AMPS), N- butoxy 2 parts of Methacrylamide (NBMA), 4 parts of acrylic acid double cyclopentenyl ester (DCPA), 2 parts of chain extender l, 4- butanediol, water 150 Part, 3 parts of crosslinking agent acrylonitrile, 1 part of sorbitan ester class surfactant, 2 parts of catalyst dibutyltin dilaurylate are mixed It closes uniformly, phosphoric acid regulation system pH value is added to 6, is passed through inert gas to remove the dissolved oxygen in reaction system;S2, by S1 institute The reaction system obtained cools to 10 DEG C, adds 2 parts of initiator azo-bis-isobutyrate hydrochloride, heating carries out polymerization reaction;S3, The jelly that the reactant that S2 is obtained obtains takes out, and after being granulated, dry, crushing, obtains polyacrylamide flocculant.
Beneficial effect
Wastewater treatment method provided by the invention can preferably be handled phosphorous and oil-containing waste water simultaneously, have technique Simply, the advantages of high treating effect.
Specific embodiment
The unit of heretofore described additional amount, such as mg/L, g/L etc. all refer to outer in no special instruction Ratio between the weight of adding medicine and the volume of waste water.
In method of the invention, the grease in waste water is decomposed by small-molecule substance by wet oxidation first, it is therefore prevented that The influence that grease reacts calcium precipitate improves precipitation reaction efficiency;In addition, preventing small molecule grease pair by ultrasonic wave added The influence of precipitation reaction enables flocculation reaction be removed more impurity.
Embodiment 1
Step 1, will contain white oil 0.1g/L, and the phosphorous oily waste water of total phosphorus (TP) concentration 0.1g/L first carries out quartz filter Pre-filtering, then handled by wet oxidation, the temperature range of wet oxidation is 125 DEG C, pressure limit is 0.5Mpa, and oxygen adds Enter 1~4g/L of amount;
The pH of feed liquid after oxidation processes is adjusted to 9 by step 2, then under conditions of ultrasonic wave added, and calcium chloride precipitation agent is added Precipitation reaction is carried out with 0.5g/L polyacrylamide flocculant, the additional amount of calcium precipitation agent and the molar ratio of total phosphorus are 2:1, are surpassed Sound condition is frequency 400kHz, ultrasonic power 1W/cm2, after removal precipitates, obtain the first feed liquid;
The pH of first feed liquid is adjusted to 3,1g/L aluminium polychloride is added by step 3, carries out flocculation precipitation reaction, removal precipitating Afterwards, the second feed liquid is obtained;
Second feed liquid is sent into reverse osmosis membrane and be filtered, obtains that treated and produce water by step 4.
The preparation method of the polyacrylamide flocculant includes the following steps: S1, by weight, in reactor Middle 35 parts of addition acrylamide monomer, 2 parts of tung oil, 3 parts of 2- acrylamido -2- methyl propane sulfonic acid (AMPS), N- butoxy 2 parts of Methacrylamide (NBMA), 4 parts of acrylic acid double cyclopentenyl ester (DCPA), 2 parts of chain extender l, 4- butanediol, water 150 Part, 3 parts of crosslinking agent acrylonitrile, 1 part of sorbitan ester class surfactant, 2 parts of catalyst dibutyltin dilaurylate are mixed It closes uniformly, phosphoric acid regulation system pH value is added to 5, is passed through inert gas to remove the dissolved oxygen in reaction system;S2, by S1 institute The reaction system obtained cools to 10 DEG C, adds 2 parts of initiator azo-bis-isobutyrate hydrochloride, heating carries out polymerization reaction;3rd The jelly that the reactant that step, S2 are obtained obtains takes out, and after being granulated, dry, crushing, obtains polyacrylamide flocculant.
Embodiment 2
Step 1, will contain white oil 5g/L, and the phosphorous oily waste water of total phosphorus (TP) concentration 3g/L first carries out the pre- of quartz filter Filtering, then by wet oxidation processing, the temperature range of wet oxidation is 220 DEG C, pressure limit is 5Mpa, oxygen additional amount 1 ~4g/L;
The pH of feed liquid after oxidation processes is adjusted to 11 by step 2, then under conditions of ultrasonic wave added, and calcium chloride precipitation is added Agent and 3g/L polyacrylamide flocculant carry out precipitation reaction, and the additional amount of calcium precipitation agent and the molar ratio of total phosphorus are 4:1, surpass Sound condition is frequency 600kHz, ultrasonic power 5W/cm2, after removal precipitates, obtain the first feed liquid;
The pH of first feed liquid is adjusted to 5,5g/L aluminium polychloride is added by step 3, carries out flocculation precipitation reaction, removal precipitating Afterwards, the second feed liquid is obtained;
Second feed liquid is sent into reverse osmosis membrane and be filtered, obtains that treated and produce water by step 4.
The preparation method of the polyacrylamide flocculant includes the following steps: S1, by weight, in reactor Middle 35 parts of addition acrylamide monomer, 2 parts of tung oil, 3 parts of 2- acrylamido -2- methyl propane sulfonic acid (AMPS), N- butoxy 2 parts of Methacrylamide (NBMA), 4 parts of acrylic acid double cyclopentenyl ester (DCPA), 2 parts of chain extender l, 4- butanediol, water 150 Part, 3 parts of crosslinking agent acrylonitrile, 1 part of sorbitan ester class surfactant, 2 parts of catalyst dibutyltin dilaurylate are mixed It closes uniformly, phosphoric acid regulation system pH value is added to 5, is passed through inert gas to remove the dissolved oxygen in reaction system;S2, by S1 institute The reaction system obtained cools to 10 DEG C, adds 2 parts of initiator azo-bis-isobutyrate hydrochloride, heating carries out polymerization reaction;3rd The jelly that the reactant that step, S2 are obtained obtains takes out, and after being granulated, dry, crushing, obtains polyacrylamide flocculant.
Embodiment 3
Step 1, will contain white oil 3g/L, and the phosphorous oily waste water of total phosphorus (TP) concentration 1g/L first carries out the pre- of quartz filter Filtering, then by wet oxidation processing, the temperature range of wet oxidation is 170 DEG C, pressure limit is 2Mpa, oxygen additional amount 2g/L;
The pH of feed liquid after oxidation processes is adjusted to 10 by step 2, then under conditions of ultrasonic wave added, and calcium chloride precipitation is added Agent and 2g/L polyacrylamide flocculant carry out precipitation reaction, and the additional amount of calcium precipitation agent and the molar ratio of total phosphorus are 3:1, surpass Sound condition is frequency 500kHz, ultrasonic power 2W/cm2, after removal precipitates, obtain the first feed liquid;
The pH of first feed liquid is adjusted to 4,2g/L aluminium polychloride is added by step 3, carries out flocculation precipitation reaction, removal precipitating Afterwards, the second feed liquid is obtained;
Second feed liquid is sent into reverse osmosis membrane and be filtered, obtains that treated and produce water by step 4.
The preparation method of the polyacrylamide flocculant includes the following steps: S1, by weight, in reactor Middle 35 parts of addition acrylamide monomer, 2 parts of tung oil, 3 parts of 2- acrylamido -2- methyl propane sulfonic acid (AMPS), N- butoxy 2 parts of Methacrylamide (NBMA), 4 parts of acrylic acid double cyclopentenyl ester (DCPA), 2 parts of chain extender l, 4- butanediol, water 150 Part, 3 parts of crosslinking agent acrylonitrile, 1 part of sorbitan ester class surfactant, 2 parts of catalyst dibutyltin dilaurylate are mixed It closes uniformly, phosphoric acid regulation system pH value is added to 5, is passed through inert gas to remove the dissolved oxygen in reaction system;S2, by S1 institute The reaction system obtained cools to 10 DEG C, adds 2 parts of initiator azo-bis-isobutyrate hydrochloride, heating carries out polymerization reaction;3rd The jelly that the reactant that step, S2 are obtained obtains takes out, and after being granulated, dry, crushing, obtains polyacrylamide flocculant.
Reference examples 1
Difference with embodiment 3 is: using ozone oxidation in step 1,40 DEG C of reaction temperature, and ozone dosage 500mg/ L。
Step 1, will contain white oil 3g/L, and the phosphorous oily waste water of total phosphorus (TP) concentration 1g/L first carries out quartz filter Pre-filtering, then by ozone oxidation, 40 DEG C of reaction temperature, ozone dosage 500mg/L;
The pH of feed liquid after oxidation processes is adjusted to 10 by step 2, then under conditions of ultrasonic wave added, and calcium chloride precipitation is added Agent and 2g/L polyacrylamide flocculant carry out precipitation reaction, and the additional amount of calcium precipitation agent and the molar ratio of total phosphorus are 3:1, surpass Sound condition is frequency 500kHz, ultrasonic power 2W/cm2, after removal precipitates, obtain the first feed liquid;
The pH of first feed liquid is adjusted to 4,2g/L aluminium polychloride is added by step 3, carries out flocculation precipitation reaction, removal precipitating Afterwards, the second feed liquid is obtained;
Second feed liquid is sent into reverse osmosis membrane and be filtered, obtains that treated and produce water by step 4.
The preparation method of the polyacrylamide flocculant includes the following steps: S1, by weight, in reactor Middle 35 parts of addition acrylamide monomer, 2 parts of tung oil, 3 parts of 2- acrylamido -2- methyl propane sulfonic acid (AMPS), N- butoxy 2 parts of Methacrylamide (NBMA), 4 parts of acrylic acid double cyclopentenyl ester (DCPA), 2 parts of chain extender l, 4- butanediol, water 150 Part, 3 parts of crosslinking agent acrylonitrile, 1 part of sorbitan ester class surfactant, 2 parts of catalyst dibutyltin dilaurylate are mixed It closes uniformly, phosphoric acid regulation system pH value is added to 5, is passed through inert gas to remove the dissolved oxygen in reaction system;S2, by S1 institute The reaction system obtained cools to 10 DEG C, adds 2 parts of initiator azo-bis-isobutyrate hydrochloride, heating carries out polymerization reaction;3rd The jelly that the reactant that step, S2 are obtained obtains takes out, and after being granulated, dry, crushing, obtains polyacrylamide flocculant.
Reference examples 2
Difference with embodiment 3 is: ultrasonic wave added not being added.
Step 1, will contain white oil 3g/L, and the phosphorous oily waste water of total phosphorus (TP) concentration 1g/L first carries out quartz filter Pre-filtering, then handled by wet oxidation, the temperature range of wet oxidation is 170 DEG C, pressure limit is 2Mpa, and oxygen is added Measure 2g/L;
The pH of feed liquid after oxidation processes is adjusted to 10 by step 2, adds calcium chloride precipitation agent and 2g/L polyacrylamide wadding Solidifying agent carries out precipitation reaction, and the additional amount of calcium precipitation agent and the molar ratio of total phosphorus are 3:1, after removal precipitating, obtains the first material Liquid;
The pH of first feed liquid is adjusted to 4,2g/L aluminium polychloride is added by step 3, carries out flocculation precipitation reaction, removal precipitating Afterwards, the second feed liquid is obtained;
Second feed liquid is sent into reverse osmosis membrane and be filtered, obtains that treated and produce water by step 4.
The preparation method of the polyacrylamide flocculant includes the following steps: S1, by weight, in reactor Middle 35 parts of addition acrylamide monomer, 2 parts of tung oil, 3 parts of 2- acrylamido -2- methyl propane sulfonic acid (AMPS), N- butoxy 2 parts of Methacrylamide (NBMA), 4 parts of acrylic acid double cyclopentenyl ester (DCPA), 2 parts of chain extender l, 4- butanediol, water 150 Part, 3 parts of crosslinking agent acrylonitrile, 1 part of sorbitan ester class surfactant, 2 parts of catalyst dibutyltin dilaurylate are mixed It closes uniformly, phosphoric acid regulation system pH value is added to 5, is passed through inert gas to remove the dissolved oxygen in reaction system;S2, by S1 institute The reaction system obtained cools to 10 DEG C, adds 2 parts of initiator azo-bis-isobutyrate hydrochloride, heating carries out polymerization reaction;3rd The jelly that the reactant that step, S2 are obtained obtains takes out, and after being granulated, dry, crushing, obtains polyacrylamide flocculant.
Reference examples 3
Difference with embodiment 3 is: N- butoxymethyl acryloyl is not added in the preparation of polyacrylamide flocculant, in S1 Amine.
Step 1, will contain white oil 3g/L, and the phosphorous oily waste water of total phosphorus (TP) concentration 1g/L first carries out quartz filter Pre-filtering, then handled by wet oxidation, the temperature range of wet oxidation is 170 DEG C, pressure limit is 2Mpa, and oxygen is added Measure 2g/L;
The pH of feed liquid after oxidation processes is adjusted to 10 by step 2, then under conditions of ultrasonic wave added, and calcium chloride precipitation is added Agent and 2g/L polyacrylamide flocculant carry out precipitation reaction, and the additional amount of calcium precipitation agent and the molar ratio of total phosphorus are 3:1, surpass Sound condition is frequency 500kHz, ultrasonic power 2W/cm2, after removal precipitates, obtain the first feed liquid;
The pH of first feed liquid is adjusted to 4,2g/L aluminium polychloride is added by step 3, carries out flocculation precipitation reaction, removal precipitating Afterwards, the second feed liquid is obtained;
Second feed liquid is sent into reverse osmosis membrane and be filtered, obtains that treated and produce water by step 4.
The preparation method of the polyacrylamide flocculant includes the following steps: S1, by weight, in reactor Middle 35 parts of addition acrylamide monomer, 2 parts of tung oil, 3 parts of 2- acrylamido -2- methyl propane sulfonic acid (AMPS), acrylic acid are double 4 parts of cyclopentene base ester (DCPA), 2 parts of chain extender l, 4- butanediol, 150 parts of water, 3 parts of crosslinking agent acrylonitrile, sorbitan 1 part of esters surface active agent, 2 parts of catalyst dibutyltin dilaurylate are uniformly mixed, addition phosphoric acid regulation system pH value to 5, Inert gas is passed through to remove the dissolved oxygen in reaction system;S2, the resulting reaction system of S1 is cooled to 10 DEG C, adds and draws 2 parts of agent azo-bis-isobutyrate hydrochloride of hair, heating carry out polymerization reaction;The jelly that the reactant that step 3, S2 are obtained obtains takes Out, after being granulated, dry, crushing, polyacrylamide flocculant is obtained.
By being investigated to the second material liquid component and reverse osmosis membrane operating condition.
As can be seen from the above table, waste water treatment process provided by the invention can be removed preferably while oil-containing and phosphorous useless Pollutant in water, embodiment 3 and reference examples 1 are compared as can be seen that wet oxidation can preferably remove grease in waste water, Prevent grease from influencing precipitating flocculation reaction;Embodiment 3 is compared with reference examples 2 as can be seen that can be improved by ultrasonic wave added Flocculation precipitation reaction effect, prevents grease from having an impact to precipitation process, improves the removal rate of total phosphorus;Embodiment 3 is relative to right 2 by the way that N- butoxy methyl acrylamide monomer is added in preparing to acrylamide flocculating agent as can be seen that can be improved as usual For the removal effect of sediment and grease.

Claims (9)

1. a kind of preparation method of polyacrylamide flocculant, which comprises the steps of:
Acrylamide monomer, tung oil, 2- acrylamido -2- methyl propane sulfonic acid is added in S1, by weight in the reactor 3 parts, N- butoxy methyl acrylamide, acrylic acid double cyclopentenyl ester, chain extender, water, crosslinking agent, 1 part of surfactant, urge Agent is uniformly mixed, and regulation system pH value is passed through inert gas to remove the dissolved oxygen in reaction system;
S2, the resulting reaction system of S1 is cooled down, adds initiator, heating carries out polymerization reaction;
The jelly that S3, the reactant for obtaining S2 obtain takes out, and after being granulated, dry, crushing, obtains polyacrylamide flocculation Agent.
2. the preparation method of polyacrylamide flocculant described in claim 1, which is characterized in that regulation system pH value is to pass through Phosphoric acid is added.
3. the preparation method of polyacrylamide flocculant according to claim 1, which is characterized in that regulation system pH value is extremely 6。
4. the preparation method of polyacrylamide flocculant according to claim 1, which is characterized in that catalyst is two laurels Sour dibutyl tin;Chain extender is l, 4- butanediol;Crosslinking agent is acrylonitrile;Surfactant is sorbitan ester class surface Activating agent;Initiator is azo-bis-isobutyrate hydrochloride.
5. the preparation method of polyacrylamide flocculant according to claim 1, which is characterized in that the additional amount of raw material is pressed Be according to parts by weight meter: preferably 35 parts of acrylamide monomer, preferably 2 parts of tung oil, 2- acrylamido -2- methyl propane sulfonic acid are preferred 3 parts, preferably 2 parts of N- butoxy methyl acrylamide, preferably 4 parts of acrylic acid double cyclopentenyl ester, preferably 2 parts of chain extender, water it is excellent Select 150 parts, preferably 3 parts of crosslinking agent, preferably 1 part of surfactant, preferably 2 parts of catalyst, preferably 2 parts of initiator.
6. the preparation method of polyacrylamide flocculant according to claim 1, which is characterized in that except temperature is cooling in S2 To 10 DEG C.
7. the obtained flocculant of preparation method described in any one of claims 1-6.
8. flocculant as claimed in claim 7 is for handling the purposes in phosphorous oily waste water.
9. phosphorous oily waste water according to claim 8,0.1~5g/ of mineral oil is contained in the phosphorous oily waste water L, 0.1~3g/L of total phosphorus (TP) concentration;The mineral oil is white oil, and the total phosphorus is by phosphate, hypophosphites, phosphorous Hydrochlorate composition.
CN201910009241.5A 2016-07-28 2016-07-28 A kind of use in waste water treatment flocculant and preparation method thereof Pending CN109502833A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910009241.5A CN109502833A (en) 2016-07-28 2016-07-28 A kind of use in waste water treatment flocculant and preparation method thereof

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201910009241.5A CN109502833A (en) 2016-07-28 2016-07-28 A kind of use in waste water treatment flocculant and preparation method thereof
CN201610604238.4A CN106007128B (en) 2016-07-28 2016-07-28 A kind of processing method of phosphorous oily waste water

Related Parent Applications (1)

Application Number Title Priority Date Filing Date
CN201610604238.4A Division CN106007128B (en) 2016-07-28 2016-07-28 A kind of processing method of phosphorous oily waste water

Publications (1)

Publication Number Publication Date
CN109502833A true CN109502833A (en) 2019-03-22

Family

ID=57115441

Family Applications (2)

Application Number Title Priority Date Filing Date
CN201910009241.5A Pending CN109502833A (en) 2016-07-28 2016-07-28 A kind of use in waste water treatment flocculant and preparation method thereof
CN201610604238.4A Active CN106007128B (en) 2016-07-28 2016-07-28 A kind of processing method of phosphorous oily waste water

Family Applications After (1)

Application Number Title Priority Date Filing Date
CN201610604238.4A Active CN106007128B (en) 2016-07-28 2016-07-28 A kind of processing method of phosphorous oily waste water

Country Status (1)

Country Link
CN (2) CN109502833A (en)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107698059A (en) * 2017-10-31 2018-02-16 惠州市宙邦化工有限公司 A kind of phosphorus-containing wastewater contamination precipitation processing method
CN110357325A (en) * 2019-07-10 2019-10-22 吉林建筑大学 A kind of processing method of oily waste water
CN110981051B (en) * 2020-03-03 2020-06-02 胜利油田盛嘉化工有限责任公司 Ultrasonic treatment method for crude oil produced water
CN113526781A (en) * 2020-04-22 2021-10-22 大连波美科技有限公司 Treatment and recycling system and process for vegetable oil saponin wastewater
CN113461202B (en) * 2021-06-24 2023-10-27 宜都兴发化工有限公司 High-phosphorus and high-calcium magnesium recycling treatment method
CN114772836B (en) * 2022-04-28 2024-02-27 青岛海纳能源环保科技开发有限公司 Treatment method of waste emulsion
CN115448501A (en) * 2022-10-20 2022-12-09 湖南天泰天润新能源科技有限公司 Dephosphorization method for waste water recovered from waste lithium iron phosphate batteries
CN116622037B (en) * 2023-07-25 2023-10-13 东明旭阳化工有限公司 Method for removing total phosphorus from caprolactam oximation wastewater, calcium hydroxide precipitant used in method and preparation method of precipitant

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE667873A (en) * 1964-08-04 1966-02-04
IT1021738B (en) * 1973-10-10 1978-02-20 Allied Colloids Ltd SYNTHETIC FLOCCULATING POLYMERS FOR ALKALINE SYSTEMS AND PROCEDURE FOR PRODUCING THEM
CN1235613A (en) * 1996-09-03 1999-11-17 帝国化学工业公司 Polyacrylamide polymerization
CN1884316A (en) * 2006-06-23 2006-12-27 张金保 Polymerization promoting initiator for producing super high molecular weight polyacrylamide and preparation method
CN101143742A (en) * 2006-09-15 2008-03-19 中国石油化工股份有限公司 Reversed phase emulsion synthesis method for polyacrylamide flocculant
CN101845115A (en) * 2010-04-28 2010-09-29 北京化工大学 Preparation method and application of water-based polyacrylamide composite dispersion liquid
CN101899129A (en) * 2010-07-22 2010-12-01 江苏江达生态科技有限公司 Preparation method of hydrophobic anion flocculant
EP2318109A1 (en) * 2008-07-31 2011-05-11 General Electric Company Methods for removing fats, oil and grease and recovering tallow from wastewater

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102627361A (en) * 2012-03-27 2012-08-08 浙江省环境保护科学设计研究院 Method and device for removing phosphorous from glyphosate production wastewater
CN104276686A (en) * 2013-07-09 2015-01-14 深圳海川环境科技有限公司 Organic matter-rich sewage treatment and disposal method
CN103991987B (en) * 2014-06-09 2016-07-06 北京碧水源环境工程有限公司 A kind of pretreatment high phosphorus waste water removes technique and the process system thereof of total phosphorus

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE667873A (en) * 1964-08-04 1966-02-04
IT1021738B (en) * 1973-10-10 1978-02-20 Allied Colloids Ltd SYNTHETIC FLOCCULATING POLYMERS FOR ALKALINE SYSTEMS AND PROCEDURE FOR PRODUCING THEM
CN1235613A (en) * 1996-09-03 1999-11-17 帝国化学工业公司 Polyacrylamide polymerization
CN1884316A (en) * 2006-06-23 2006-12-27 张金保 Polymerization promoting initiator for producing super high molecular weight polyacrylamide and preparation method
CN101143742A (en) * 2006-09-15 2008-03-19 中国石油化工股份有限公司 Reversed phase emulsion synthesis method for polyacrylamide flocculant
EP2318109A1 (en) * 2008-07-31 2011-05-11 General Electric Company Methods for removing fats, oil and grease and recovering tallow from wastewater
CN101845115A (en) * 2010-04-28 2010-09-29 北京化工大学 Preparation method and application of water-based polyacrylamide composite dispersion liquid
CN101899129A (en) * 2010-07-22 2010-12-01 江苏江达生态科技有限公司 Preparation method of hydrophobic anion flocculant

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
云南科技学术交流中心等: "《科技学术论文集 2007》", 31 July 2007, 原子能出版社 *
杨旭: "《中国科技发展精典文库 2003卷 中》", 31 May 2003 *

Also Published As

Publication number Publication date
CN106007128B (en) 2019-04-12
CN106007128A (en) 2016-10-12

Similar Documents

Publication Publication Date Title
CN106007128B (en) A kind of processing method of phosphorous oily waste water
CN104098228B (en) A kind of organic amine wastewater treatment process
CN103121772B (en) A kind of processing method of phosphorus-containing wastewater
CN100497193C (en) High polymer composite coagulant for treatment of oily waste water and making method thereof
CN109574394B (en) Fracturing flowback fluid treatment method
CN105174661B (en) A kind of acid washing phosphorization waste water treatment process
CN109293163A (en) A kind of composite dephosphorizing agent and application method
CN107986570A (en) A kind of leather waste water processing method
CN105906164A (en) Method for removing ammonia nitrogen in waste water
KR101278230B1 (en) The method and Appuratus of removing total nitrogen and phosphate in sewage and wastewater using precipitation-agent of rapidity for coagulation an flocculation
CN102718295A (en) Compound medicament for treating coking wastewater and preparation method thereof
CN108358270A (en) A kind of chemistry in water treatment medicament and preparation method thereof
Mohammed et al. Phosphorus removal from water and waste water by chemical precipitation using alum and calcium chloride
JP2009072769A (en) Sewage treatment system
CN105712564A (en) Equipment for processing waste water through glyphosate production
CN110615485B (en) Continuous production method and application of polyferric chloride
CN104803511A (en) High ammonia-nitrogen wastewater treatment device and treatment method
CN111018176A (en) Demulsifier, preparation method and application thereof
CN107963709A (en) A kind of high-efficiency sewage dephosphorization agent and its application in municipal wastewater advanced treating
JPH0338204A (en) Treating technique for low concentration turbid water
KR101088148B1 (en) Electrical neutralization of colloidal particles with speed control how water
WO2009156252A1 (en) Process for reducing bulking sludge in activated sludge wastewater treatment
JP2009056346A (en) Polluted muddy water treatment system
Amjad Influence of surfactants on the performance of calcium phosphate scale inhibitors
CN106362597A (en) Film-method reclaimed-water-reusing scaling inhibitor and preparing method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20190322