EP0468991A1 - Procede pour separer des emulsions d'huile dans l'eau - Google Patents

Procede pour separer des emulsions d'huile dans l'eau

Info

Publication number
EP0468991A1
EP0468991A1 EP19900905520 EP90905520A EP0468991A1 EP 0468991 A1 EP0468991 A1 EP 0468991A1 EP 19900905520 EP19900905520 EP 19900905520 EP 90905520 A EP90905520 A EP 90905520A EP 0468991 A1 EP0468991 A1 EP 0468991A1
Authority
EP
European Patent Office
Prior art keywords
oil
emulsion
water
cationic polymer
added
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
EP19900905520
Other languages
German (de)
English (en)
Inventor
Haluk Akyel
Alfons Landscheidt
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.)
Stockhausen GmbH and Co KG
Original Assignee
Chemische Fabrik Stockhausen GmbH
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 Chemische Fabrik Stockhausen GmbH filed Critical Chemische Fabrik Stockhausen GmbH
Publication of EP0468991A1 publication Critical patent/EP0468991A1/fr
Pending legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02—Separation of non-miscible liquids
    • B01D17/04—Breaking emulsions
    • B01D17/047—Breaking emulsions with separation aids
    • 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
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material

Definitions

  • the invention relates to a method for separating oil / water emulsions.
  • Oil / water emulsions often occur as contaminated product streams, which in addition to organic substances such as Mineral oils, vegetable oils, animal oils or fats in emulsified form also contain those in non-emulsified form and solid particles.
  • wastewater contaminated with oil or grease is often produced, which belongs to the group of heavily polluted wastewater and represents major problems for sewage treatment plants . It is therefore imperative to purify such wastewater beforehand using special methods and to discharge it into the receiving water or sewage treatment plants only after such a pre-treatment stage.
  • emulsion splitting the organic phase present in the water emulsified must be converted into the "free" form.
  • emulsion splitting This process is referred to as "emulsion splitting".
  • the emulsion must first be broken for physical liquid-liquid phase separation. In the case of unstable emulsions, prolonged standing and / or heating can lead to phase separation.
  • the emulsions stabilized with emulsifiers must be treated with chemical agents for the cleavage in order to largely discharge the very fine organic liquid particles which are electrostatically charged in the aqueous phase. In this case, the mutual repulsive forces between the organic particles emulsified in the water are eliminated, and the fine droplets are agglomerated and the emulsion is ultimately split by increasing the size of the drops.
  • Oil particles in an aqueous emulsion are usually negatively charged.
  • cations are added to the emulsion.
  • organic water-soluble cationic polymers with different chain lengths or molecular weights are also used as emulsion breakers for the same purpose.
  • Both cationic and anionic water-soluble polymers are often used in combination with iron or aluminum salts for cleaning oil-containing wastewater.
  • Corresponding cleaning methods are generally used in practice in flotation plants of various types, e.g. Relaxation flotation, mechanical flotation, etc. carried out.
  • DE-0S 19 26 623 describes a method for separating oil from stable oil-in-water emulsions, in which the emulsion is mixed with an iron salt and sodium hydroxide solution and then treated with a high molecular weight, water-soluble polymer based on polyacrylic acid, polyacrylamide, polyvinyl alcohol and polyethylene oxide.
  • DE-OS 28 41 122 describes the use of cationic, anionic or nonionic polymers alone or in combination with metal salts for wastewater treatment.
  • Cationic polymer types are polyamides, polyamines and copolymers of acrylamide with quaternary ammonium polyacrylamides.
  • US Pat. No. 3,691,086 describes a process using cationic polymers for oil / water separation, in which the polymers are preferably used in conjunction with a silica sol and a polyvalent metal salt. Polymers according to this US Pat. No. 3,691,086 are compared in Comparative Examples AF with the polymers according to the invention, in order to show that a better qualitative and quantitative separation is obtained with the products according to the invention.
  • the object of the present invention is to complete the emulsion splitting effect by providing an improved emulsion splitting agent and to provide a process which leads to a satisfactory separation effect both in flotation plants and in static separation devices.
  • R2 a straight chain or branched
  • R5 is an alkylene aromatic residue X mean C1-, CH3S04 ⁇ ,
  • acrylamide 20 to 95% acrylamide and c) 0 to 10% of another water soluble monomer e.g. Methacrylamide, (meth) acrylic acid, vinylpyrrolidone, dimethyldiallylammonium chloride, acrylamidomethylpropanesulfonic acid, N, N-dimethylacrylamide, vinyl acetamide or vinyl formamide.
  • another water soluble monomer e.g. Methacrylamide, (meth) acrylic acid, vinylpyrrolidone, dimethyldiallylammonium chloride, acrylamidomethylpropanesulfonic acid, N, N-dimethylacrylamide, vinyl acetamide or vinyl formamide.
  • a cationic polymer of the abovementioned composition By adding a cationic polymer of the abovementioned composition in an amount of 0.1 to 50% by weight, preferably 1 to 20% by weight, based on the organic portion of the oil / water emulsion, this is split Oil / water emulsion reached.
  • the cationic polymer can be added to the oil / water emulsion to be cleaved in the form of an emulsion, in powder form or in the form of an aqueous solution.
  • the third water-soluble monomer component c) can preferably be acrylic acid or N-vinylpyrrolidone.
  • Comparative product A copolymer consisting of
  • N- (dimethylamino-propyl) acrylamide 25% by weight of N- (dimethylamino-propyl) acrylamide, quaternized with methyl chloride and 75% by weight of acrylamide.
  • Comparative product B copolymer consisting of
  • Product B copolymer consisting of 70% by weight of N- (dimethylamino-propyl) -acrylamide, quaternized with benzyl chloride and 30% by weight of acrylamide.
  • Comparative product C copolymer consisting of
  • Product C copolymer consisting of 5% by weight dimethylaminoethyl acrylate, quaternized with benzyl chloride and 95% by weight acrylamide.
  • Comparative product D copolymer consisting of
  • Product D copolymer consisting of 50% by weight dimethylamino-2,2-dimethylpropyl acrylamide, quater nized with benzyl chloride and 50 wt .-% acrylamide.
  • Comparative product E polymer consisting of
  • Comparative product F polymer consisting of
  • the residual oil contents in the purified water were determined as non-volatile lipophilic substances according to DIN 38409, part H Iß.
  • the wastewater was mixed in a beaker with 50 ppm each of the aforementioned comparison products or products.
  • the emulsion breakers were added from a 0.1% aqueous solution.
  • the samples were stirred for 60 seconds with a finger stirrer at 50 rpm. During this time the emulsion was split, the organic phase settled on the water surface when it was left to stand for 30 minutes.
  • the determination of the residual oil contents as lipophilic substances with low volatility was carried out for the lower aqueous phase.
  • Example 2 (test series 2, flotation)
  • the wastewater was placed in a 2 liter laboratory flotation cell, type KHD.
  • a 2 liter laboratory flotation cell type KHD.
  • 5 ppm of emulsion breakers from a 0.1% strength aqueous solution were added and then floated for 5 minutes.
  • the organic matter discharged with the foam was separated from the flotation cell using a scraper.
  • the purified water was examined as described in accordance with DIN 38409, part H 18.
  • test results with the comparative products E and F show that quaternized homopolymers, both with and without benzyl grouping, give significantly poorer separation results than the copolymers used according to the invention.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Hydrology & Water Resources (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Fats And Perfumes (AREA)

Abstract

Procédé pour séparer des émulsions d'huile dans l'eau en y ajoutant des polymères cationiques. On ajoute à l'émulsion à séparer un polymère organique cationique synthétique comportant (a) 5 à 70 % en poids d'un monomère correspondant à la formule générale (I), où R1 représente -H ou -CH3; Y représente -O- ou -NH-; R2 représente un groupe alkylène linéaire ou ramifié avec 2 à 6 atomes de C; R3 et R4 représentent -CH3 ou -CH2-CH3; R5 représente un résidu alkylène aromatique; et X représente Cl-, CH3SO4-; (b) 20 à 95 % d'acrylamide; et (c) 0 à 10 % d'un autre monomère soluble dans l'eau.
EP19900905520 1989-04-20 1990-04-12 Procede pour separer des emulsions d'huile dans l'eau Pending EP0468991A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3912929 1989-04-20
DE19893912929 DE3912929A1 (de) 1989-04-20 1989-04-20 Mittel und verfahren zur spaltung von oel/wasser-emulsionen

Publications (1)

Publication Number Publication Date
EP0468991A1 true EP0468991A1 (fr) 1992-02-05

Family

ID=6379026

Family Applications (2)

Application Number Title Priority Date Filing Date
EP90107042A Withdrawn EP0398022A1 (fr) 1989-04-20 1990-04-12 Procédé de séparation d'émulsions l'huile dans l'eau
EP19900905520 Pending EP0468991A1 (fr) 1989-04-20 1990-04-12 Procede pour separer des emulsions d'huile dans l'eau

Family Applications Before (1)

Application Number Title Priority Date Filing Date
EP90107042A Withdrawn EP0398022A1 (fr) 1989-04-20 1990-04-12 Procédé de séparation d'émulsions l'huile dans l'eau

Country Status (6)

Country Link
EP (2) EP0398022A1 (fr)
JP (1) JP2745244B2 (fr)
CA (1) CA2053227A1 (fr)
DE (1) DE3912929A1 (fr)
GR (1) GR910300036T1 (fr)
WO (1) WO1990012633A1 (fr)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5330650A (en) * 1992-10-30 1994-07-19 Nalco Chemical Company Dispersion polymers for oil field water clarification
KR100216494B1 (ko) * 1993-03-01 1999-08-16 로날드 제이. 알레인, 지이 엠 브랜논, 더블유 이 패리 수용성 양이온성 중합체 분산액을 사용하여 폐액으로부터 오일을 회수하고 산업 폐수로부터 오일을 제거하는 방법
FR2707288B1 (fr) * 1993-07-05 1995-09-01 Atochem Elf Sa Chlorure de méthacrylate de tertiobutylaminoéthyle, son procédé de préparation et ses applications.
CN1208110C (zh) 2000-10-13 2005-06-29 日本阿尔西株式会社 油水分离絮凝剂及油水分离絮凝方法

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3691086A (en) * 1970-07-31 1972-09-12 Hercules Inc Oil-water separations
US4179549A (en) * 1974-11-14 1979-12-18 Petrolite Corporation Quaternary ammonium adducts of polymerizable tertiary ammonium salts and acrylamide
US4160742A (en) * 1978-06-15 1979-07-10 Calgon Corporation Method of resolving oil-in-water emulsions
US4454047A (en) * 1981-03-09 1984-06-12 Petrolite Corporation Process of treating aqueous systems
US4444971A (en) * 1983-07-25 1984-04-24 Texaco Inc. Acrylic and methacrylic quaternary chloromethyl ammonium chloride cationic monomers and polymers thereof
US4734205A (en) * 1986-09-08 1988-03-29 Exxon Research And Engineering Company Hydrophobically associating polymers for oily water clean-up

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO9012633A1 *

Also Published As

Publication number Publication date
JPH04504675A (ja) 1992-08-20
JP2745244B2 (ja) 1998-04-28
EP0398022A1 (fr) 1990-11-22
GR910300036T1 (en) 1991-11-15
WO1990012633A1 (fr) 1990-11-01
CA2053227A1 (fr) 1990-10-21
DE3912929C2 (fr) 1993-08-26
DE3912929A1 (de) 1990-10-31

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