US20020190007A1 - Flocculant for oil-water separation and method for oil-water separation by flocculation - Google Patents
Flocculant for oil-water separation and method for oil-water separation by flocculation Download PDFInfo
- Publication number
- US20020190007A1 US20020190007A1 US10/148,735 US14873502A US2002190007A1 US 20020190007 A1 US20020190007 A1 US 20020190007A1 US 14873502 A US14873502 A US 14873502A US 2002190007 A1 US2002190007 A1 US 2002190007A1
- Authority
- US
- United States
- Prior art keywords
- water
- group
- flocculant
- oil
- components
- 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.)
- Abandoned
Links
- 0 *C([3*])(C)C([1*])([2*])C.[4*]C([5*])(C)C([6*])(C)[Y].[7*]C([8*])(C)C([9*])(C)C Chemical compound *C([3*])(C)C([1*])([2*])C.[4*]C([5*])(C)C([6*])(C)[Y].[7*]C([8*])(C)C([9*])(C)C 0.000 description 3
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/32—Materials not provided for elsewhere for absorbing liquids to remove pollution, e.g. oil, gasoline, fat
-
- 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
-
- 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
- C02F1/40—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
- 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
- C02F1/5272—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using specific organic precipitants
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/34—Esters containing nitrogen, e.g. N,N-dimethylaminoethyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/34—Esters containing nitrogen, e.g. N,N-dimethylaminoethyl (meth)acrylate
- C08F220/36—Esters containing nitrogen, e.g. N,N-dimethylaminoethyl (meth)acrylate containing oxygen in addition to the carboxy oxygen, e.g. 2-N-morpholinoethyl (meth)acrylate or 2-isocyanatoethyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G33/00—Dewatering or demulsification of hydrocarbon oils
- C10G33/04—Dewatering or demulsification of hydrocarbon oils with chemical means
-
- 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
- C02F1/56—Macromolecular 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
- C02F2101/30—Organic 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
- C02F2101/30—Organic compounds
- C02F2101/32—Hydrocarbons, e.g. oil
Definitions
- oil components and “water components” herein mean components in an oily layer, and components in a water layer of the emulsion that contains oil, water, a surfactant, a stabilizer, and contaminants, respectively.
- a non-ionic surfactant is added to the mixture of the compound represented by the general formula R 0 —Q, and the compound having at least a cationic group.
- cationic group herein means a group having a quaternary nitrogen atom and an electrophilic group.
- the unit (i) for use in the present invention includes an —SO 3 M group, wherein M is hydrogen or a metal element.
- the —SO 3 M group is bonded at an end of a side chain of the polymer.
- the metal element is preferably an alkali metal element that render water solubility to the flocculant, i.e., Na, K, and Li.
- Examples of the —SO 3 M group include —C 6 H 6 SO 3 H—, —CONHCH 2 CH 2 C(CH 3 ) 2 CH 2 SO 3 H, —CONHCH 2 C(CH 3 ) 2 CH 2 SO 3 H, and —CONHC(CH 3 ) 2 CH 2 SO 3 H.
- the unit (ii) is formed by adding a monomer including the group having a quaternary nitrogen atom upon polymerization.
- a monomer including the group having a quaternary nitrogen atom upon polymerization examples include acrylic acid dimethylaminoethylmethylchloride monomer, and methacrylate acid dimethylaminoethylmethylchloride monomer.
- the flocculant for separating and flocculating oily components and water components according to the present invention may comprise a copolymer in which a unit represented by the following formula in the polymer chain.
- R 10 is hydrogen or a lower alkyl group
- R 11 is a carboxyl group, an alkoxyl group, an amino group, a group having these groups at an end, or a derivative thereof.
- the —OSO 3 M group may be not only at the molecular end, but also be in the molecular chain as a side chain.
- a compound having a double bond in its main chain as the units is used and reacted with peroxodisulfuric acid salt, i.e., potassium peroxodisulfate or sulfuric acid at the double bond. It is preferable that about equimolar amounts of peroxodisulfuric acid salt, i.e., potassium peroxodisulfate be reacted.
- the R 0 is a hydrocarbon having at least an unsaturated linking in a molecule, and a residue group of the unsaturated linking of a derivative thereof.
- Such a polymer has a molecular weight so that activity of the active sludge is not prohibited in the secondary treatment. If the molecular weight is too low, the cationic group develops a bactericidal property, and the active sludge may be destroyed. It is preferable that the compound having the cationic group have the ultimate viscosity of 0.001 to 0.6 dl/g.
- the flocculant according to the present invention was prepared as follows:
- the flocculant according to the present invention was prepared as follows:
- the flocculant according to the present invention was prepared as EXAMPLE 3 except that 5 liters aqueous solution containing 0.2 mol of potassium peroxodisulfate (K 2 S 2 O 8 ) was used. The mixture was reacted at 50° C. for 8 hours. The resulting reaction product was dropped into a large quantity of acetone to produce a white powder polymer. The polymer was dissolved in a 2 mol/l KBr aqueous solution at the concentration of 0.5 g/l. Then, the polymer was measured for ultimate viscosity at 25° C. The ultimate viscosity of the polymer was 0.12 dl/g. The polymer had an —OSO 3 K group at an end of the molecule, and an —SO 3 H group and a cationic group having a quaternary nitrogen atom at a side chain of the molecule.
- K 2 S 2 O 8 potassium peroxodisulfate
- the flocculant according to the present invention was prepared as follows:
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Health & Medical Sciences (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Thermal Sciences (AREA)
- Physics & Mathematics (AREA)
- Public Health (AREA)
- Materials Engineering (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US12/316,616 US7618540B2 (en) | 2000-10-13 | 2008-12-15 | Flocculant for separating and flocculating oil and water |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000-313682 | 2000-10-13 | ||
| JP2000313682 | 2000-10-13 |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US12/316,616 Continuation US7618540B2 (en) | 2000-10-13 | 2008-12-15 | Flocculant for separating and flocculating oil and water |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US20020190007A1 true US20020190007A1 (en) | 2002-12-19 |
Family
ID=18793059
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US10/148,735 Abandoned US20020190007A1 (en) | 2000-10-13 | 2001-10-12 | Flocculant for oil-water separation and method for oil-water separation by flocculation |
| US12/316,616 Expired - Fee Related US7618540B2 (en) | 2000-10-13 | 2008-12-15 | Flocculant for separating and flocculating oil and water |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US12/316,616 Expired - Fee Related US7618540B2 (en) | 2000-10-13 | 2008-12-15 | Flocculant for separating and flocculating oil and water |
Country Status (6)
| Country | Link |
|---|---|
| US (2) | US20020190007A1 (fr) |
| EP (1) | EP1329250B9 (fr) |
| JP (1) | JP4171648B2 (fr) |
| KR (1) | KR100855164B1 (fr) |
| CN (1) | CN1208110C (fr) |
| WO (1) | WO2002032538A1 (fr) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN119192671A (zh) * | 2024-10-15 | 2024-12-27 | 云浮市润澳新材料科技有限公司 | 一种静脉化产业树脂废弃溶剂循环利用方法 |
| WO2025024429A1 (fr) * | 2023-07-25 | 2025-01-30 | Basf Corporation | Procédés de séparation de phase aqueuse d'une émulsion |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3092047B1 (fr) * | 2014-01-09 | 2018-03-28 | Dow Global Technologies LLC | Composition et procédé pour processus de clarification d'eau de champs petroliferes |
| CN113929638A (zh) * | 2021-12-16 | 2022-01-14 | 山东尚科环境工程有限公司 | 一种噁唑烷类络合物、制备方法及其在油田污水处理中的应用 |
Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4127500A (en) * | 1976-07-19 | 1978-11-28 | Teijin Limited | Fibrous material for emulsion breaker and method for manufacturing it |
| US4182690A (en) * | 1976-11-16 | 1980-01-08 | Teijin Limited | Emulsion breaking material |
| US4305860A (en) * | 1980-08-21 | 1981-12-15 | National Starch And Chemical Corporation | Stable, pumpable, solvent-free colloidal polyampholyte latices, their preparation and use in paper |
| US4451628A (en) * | 1982-09-13 | 1984-05-29 | Celanese Corporation | Process for preparing low molecular weight water-soluble polymers by copolymerizing with water-soluble monomers a calculated quantity of methallylsulfonate monomer |
| US4569768A (en) * | 1983-10-07 | 1986-02-11 | The Dow Chemical Company | Flocculation of suspended solids from aqueous media |
| US4590249A (en) * | 1983-10-19 | 1986-05-20 | Societe Francaise Hoechst | Cationic ampholytic tetrapolymers and cosmetic compositions containing them |
| US4608425A (en) * | 1985-01-02 | 1986-08-26 | Exxon Research And Engineering Co. | High charge density polymeric complexes - viscosifiers for acid, base and salt (aqueous) solutions |
| US4652623A (en) * | 1984-11-23 | 1987-03-24 | Calgon Corporation | Polymers for use as filtration control aids in drilling muds |
| US4959432A (en) * | 1986-05-19 | 1990-09-25 | Union Carbide Chemicals And Plastics Company Inc. | Acid viscosifier compositions |
| US5308499A (en) * | 1989-05-22 | 1994-05-03 | Commonwealth Scientific And Industrial Research Organisation | Effluent treatment |
| US5354481A (en) * | 1988-12-19 | 1994-10-11 | Cytec Technology Corp. | Water-soluble highly branched polymeric microparticles |
| US5879670A (en) * | 1997-03-31 | 1999-03-09 | Calgon Corporation | Ampholyte polymers for use in personal care products |
| US5883181A (en) * | 1993-11-24 | 1999-03-16 | Cytec Technology Corp. | Multimodal emulsions and processes for preparing multimodal emulsions |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5261356A (en) | 1975-11-14 | 1977-05-20 | Toray Ind Inc | Disposing method of water containing surface active agent |
| JPS5311183A (en) | 1976-07-19 | 1978-02-01 | Teijin Ltd | Treating material for emulsifiable compounds |
| JPS5361575A (en) | 1976-11-16 | 1978-06-02 | Teijin Ltd | Treating material for emulsoidal compounds |
| JPS63221810A (ja) * | 1987-03-10 | 1988-09-14 | Matsumoto Yushi Seiyaku Kk | エマルジヨン破壊剤 |
| JP2721970B2 (ja) | 1988-04-28 | 1998-03-04 | 利行 今井 | 高分子凝集剤 |
| DE3912929A1 (de) * | 1989-04-20 | 1990-10-31 | Stockhausen Chem Fab Gmbh | Mittel und verfahren zur spaltung von oel/wasser-emulsionen |
| JPH02298304A (ja) | 1989-05-11 | 1990-12-10 | Sanyo Chem Ind Ltd | 高分子凝集剤 |
| JPH07232005A (ja) | 1994-02-22 | 1995-09-05 | Japan Synthetic Rubber Co Ltd | 凝集剤 |
| FR2761366A1 (fr) * | 1997-03-26 | 1998-10-02 | Synthron | Nouveaux copolymeres greffes amphoteres a biodegradabilite amelioree utilisables comme agents dispersants |
| JP4033946B2 (ja) | 1997-07-21 | 2008-01-16 | 日本アルシー株式会社 | 凝集剤および凝集方法 |
-
2001
- 2001-10-12 WO PCT/JP2001/008962 patent/WO2002032538A1/fr not_active Ceased
- 2001-10-12 JP JP2002535772A patent/JP4171648B2/ja not_active Expired - Fee Related
- 2001-10-12 EP EP01974808.6A patent/EP1329250B9/fr not_active Expired - Lifetime
- 2001-10-12 CN CNB01803120XA patent/CN1208110C/zh not_active Expired - Fee Related
- 2001-10-12 US US10/148,735 patent/US20020190007A1/en not_active Abandoned
- 2001-10-12 KR KR1020027007487A patent/KR100855164B1/ko not_active Expired - Fee Related
-
2008
- 2008-12-15 US US12/316,616 patent/US7618540B2/en not_active Expired - Fee Related
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4127500A (en) * | 1976-07-19 | 1978-11-28 | Teijin Limited | Fibrous material for emulsion breaker and method for manufacturing it |
| US4182690A (en) * | 1976-11-16 | 1980-01-08 | Teijin Limited | Emulsion breaking material |
| US4305860A (en) * | 1980-08-21 | 1981-12-15 | National Starch And Chemical Corporation | Stable, pumpable, solvent-free colloidal polyampholyte latices, their preparation and use in paper |
| US4451628A (en) * | 1982-09-13 | 1984-05-29 | Celanese Corporation | Process for preparing low molecular weight water-soluble polymers by copolymerizing with water-soluble monomers a calculated quantity of methallylsulfonate monomer |
| US4569768A (en) * | 1983-10-07 | 1986-02-11 | The Dow Chemical Company | Flocculation of suspended solids from aqueous media |
| US4590249A (en) * | 1983-10-19 | 1986-05-20 | Societe Francaise Hoechst | Cationic ampholytic tetrapolymers and cosmetic compositions containing them |
| US4652623A (en) * | 1984-11-23 | 1987-03-24 | Calgon Corporation | Polymers for use as filtration control aids in drilling muds |
| US4608425A (en) * | 1985-01-02 | 1986-08-26 | Exxon Research And Engineering Co. | High charge density polymeric complexes - viscosifiers for acid, base and salt (aqueous) solutions |
| US4959432A (en) * | 1986-05-19 | 1990-09-25 | Union Carbide Chemicals And Plastics Company Inc. | Acid viscosifier compositions |
| US5354481A (en) * | 1988-12-19 | 1994-10-11 | Cytec Technology Corp. | Water-soluble highly branched polymeric microparticles |
| US5308499A (en) * | 1989-05-22 | 1994-05-03 | Commonwealth Scientific And Industrial Research Organisation | Effluent treatment |
| US5883181A (en) * | 1993-11-24 | 1999-03-16 | Cytec Technology Corp. | Multimodal emulsions and processes for preparing multimodal emulsions |
| US5879670A (en) * | 1997-03-31 | 1999-03-09 | Calgon Corporation | Ampholyte polymers for use in personal care products |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2025024429A1 (fr) * | 2023-07-25 | 2025-01-30 | Basf Corporation | Procédés de séparation de phase aqueuse d'une émulsion |
| CN119192671A (zh) * | 2024-10-15 | 2024-12-27 | 云浮市润澳新材料科技有限公司 | 一种静脉化产业树脂废弃溶剂循环利用方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| JPWO2002032538A1 (ja) | 2004-02-26 |
| WO2002032538A1 (fr) | 2002-04-25 |
| EP1329250A1 (fr) | 2003-07-23 |
| KR100855164B1 (ko) | 2008-08-29 |
| CN1392800A (zh) | 2003-01-22 |
| JP4171648B2 (ja) | 2008-10-22 |
| EP1329250B9 (fr) | 2013-05-29 |
| KR20020070318A (ko) | 2002-09-05 |
| EP1329250B1 (fr) | 2013-01-30 |
| EP1329250A4 (fr) | 2005-01-19 |
| US7618540B2 (en) | 2009-11-17 |
| US20090105355A1 (en) | 2009-04-23 |
| CN1208110C (zh) | 2005-06-29 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| AS | Assignment |
Owner name: JAPAN ALSI CO., LTD., JAPAN Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNOR:FUJINO, KIYOHARU;REEL/FRAME:013166/0401 Effective date: 20020527 |
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| STCB | Information on status: application discontinuation |
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