WO2014046979A1 - Process for filtration enhancement of aqueous dispersions - Google Patents

Process for filtration enhancement of aqueous dispersions Download PDF

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Publication number
WO2014046979A1
WO2014046979A1 PCT/US2013/059694 US2013059694W WO2014046979A1 WO 2014046979 A1 WO2014046979 A1 WO 2014046979A1 US 2013059694 W US2013059694 W US 2013059694W WO 2014046979 A1 WO2014046979 A1 WO 2014046979A1
Authority
WO
WIPO (PCT)
Prior art keywords
polymer
group
filtration
meth
acid
Prior art date
Application number
PCT/US2013/059694
Other languages
English (en)
French (fr)
Inventor
Michael J. BLUEMLE
Lawrence J. ANDERMANN
Jeffrey H. Peltier
Original Assignee
Hercules Incorporated
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 Hercules Incorporated filed Critical Hercules Incorporated
Priority to EP13839337.6A priority Critical patent/EP2897707A4/en
Priority to AU2013318334A priority patent/AU2013318334B2/en
Priority to CN201380048874.8A priority patent/CN104640612A/zh
Priority to CA2883633A priority patent/CA2883633C/en
Priority to BR112015005846-9A priority patent/BR112015005846B1/pt
Priority to MX2015003298A priority patent/MX2015003298A/es
Publication of WO2014046979A1 publication Critical patent/WO2014046979A1/en
Priority to ZA2015/02608A priority patent/ZA201502608B/en

Links

Classifications

    • 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D21/00Separation of suspended solid particles from liquids by sedimentation
    • B01D21/01Separation of suspended solid particles from liquids by sedimentation using flocculating 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
    • 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
    • C02F1/5263Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using natural chemical compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/10Nature of the water, waste water, sewage or sludge to be treated from quarries or from mining activities

Definitions

  • the invention relates to compositions and methods which enhance the filtration of aqueous dispersions.
  • a filtration aid promoter and synthetic polymer for example, in dewatering aqueous mineral slurries by adding a filtration aid promoter and synthetic polymer to the aqueous dispersion prior to filtration.
  • the method enhances filtration when the filtration aid promoter and synthetic polymer are added prior to and/or during separation of solids phase from liquid phase in an aqueous slurry but prior to the filtration of the concentrated aqueous phase.
  • the compositions and methods have particular application with respect to mining slurries.
  • the mineral slurry may be dewatered in a two step method comprising liquid solid separation, such as in a gravity thickener, clarifier and/or hydrocyclone, which produces a liquid phase, supernatant, and a concentrate or underflow.
  • the concentrate or underflow comprises the valuable minerals which require further dewatering which occurs in a second step in which the concentrate or underflow is filtered, such as through vacuum filtration and/or pressure filtration.
  • Mw is the weight average molecular weight as determined by SEC-MALLS analysis.
  • MALLS shall mean and refer to multi- angular laser light scattering.
  • SEC-MALLS shall mean and refer to a size exclusion chromatography technique using MALLS to determine Mw.
  • the invention pertains to compositions comprising filtration aid promoters and synthetic polymer. These compositions are applied in methods for separating solids from liquids in aqueous dispersions comprising a filtration step.
  • the filtration aid and synthetic polymer are added to the aqueous dispersion prior to and/or during the physical separation of a solid phase from a liquid phase, such as allowing the solids to settle from the dispersion.
  • the solid phase may then be filtered.
  • Filtration aid promoters include at least one of natural polymers, semi-natural polymers or coagulants. Combinations of such may be used.
  • the composition is applied in dewatering processes in mining operations.
  • dewatering processes generally comprise two steps, the first step involving liquid solid separation and the second separate step involving filtration of concentrate or underflow from the liquid solid separation step.
  • the liquid solid separation is typically accomplished with gravity thickeners, clarifiers, hydrocyclones and the like. Filtration is generally accomplished by vacuum filtration, pressure filtration and the like.
  • the filtration aid promoter and synthetic polymer are added to a mineral slurry prior to the liquid solid separation step, during the liquid solid separation step or both during and prior to the liquid solid separation step.
  • the liquid solid separation step produces concentrate or underflow which requires further dewatering through a separate filtration step.
  • the combination of the filtration aid promoter and synthetic polymer when applied prior to and/or during the liquid solid separation step in mining operations increases the production of the filter cakes resulting from the separate filtration step.
  • the natural polymers that can be used for the filtration aid promoter are polysaccharides, such as potato starch, xanthan gums, guars, dextran, cellulose derivatives and glycosaminoglycans.
  • the poiydispersity index (“PDI") of the polysaccharide is from about 1.0 to about 10.0, more typically from about 1 :1 to about 9.0, and most typically from about 1.2 to about 8.0.
  • the natural polymer preferably comprises dextran, which is generally available from various suppliers. Dextran having a w of from about 5,000 to about 40,000,000, preferably from about 50,000 to about 25,000,000 and more preferably from about 200,000 to about 10,000,000, may be used. Persons of ordinary skill in these arts, after reading this disclosure, will appreciate that all ranges and values within these explicitly stated ranges are contemplated.
  • the semi-natural polymers include !ignosulfonates, such as calcium lignosuifonate, and chemically modified polysaccharides. Modified
  • polysaccharides typically useful in the process include modified starches, such as cationic starch; modified guar gum, such as cationic guar gum; and modified celluloses such as anionic carboxymethyl cellulose and hydroxyethyl cellulose. Combinations of semi-natural polymers may be used.
  • the coagulant is typically selected from an inorganic coagulant, organic coagulant and combinations thereof.
  • Inorganic coagulants include aluminum sulfate, aluminum chloride, poiyaluminum chloride, aluminum chlorohydrate, ferric chloride, ferric sulfate, ferrous sulfate and sodium aluminate.
  • Organic coagulants include polymers formed from the monomers diallyl dimethyl ammonium chloride, ethylene imine and the comonomers of epichlorohydrin and dimethylamine.
  • Inorganic coagulants also include cationically-modified tannins and melamine formaldehyde. Such coagulants include CHARGEPAC® 60, CHARGEPAC® 7 and AMERSEP® 5320, all available from Ashland.
  • Synthetic polymers include water-soluble anionic, cationic, nonionic and amphoteric polymers.
  • synthetic polymer shall include copolymers and terpolymers, as well as homopolymers.
  • the synthetic polymer has a Mw of from about 40,000 to about 25,000,000, and persons of ordinary skill in these arts, after reading this disclosure, will appreciate that all ranges and values within these explicitly stated ranges are contemplated.
  • the synthetic polymer may be linear, branched, or cross-linked. Typically, the synthetic polymer functions as a flocculant.
  • Nonionic polymers include polymers formed from one or more water soluble ethylenically unsaturated nonionic monomers, for instance acrylamide, methacrylamide, hydroxyethyl acrylate and N-vinylpyrrolidone, preferably acrylamide. Nonionic polymers also include alkoxylated multifunctional alcohols.
  • Cationic polymers are formed from one or more ethylenically unsaturated cationic monomers optionally with one or more of the nonionic monomers mentioned previously.
  • the cationic polymer may also be amphoteric provided such that there are predominantly more cationic groups than anionic groups.
  • the cationic monomers include diaikylamino alkyl (meth) acrylates, dialkylamino alkyl (meth) acrylamides, and diallyl dimethyl ammonium chloride, including acid addition and quaternary ammonium salts thereof.
  • Typical cationic monomers include the methyl chloride quaternary ammonium salts of dimethylamino ethyl acrylate and dimethyl aminoethyl methacrylate.
  • ADAME dimethylamino ethyl acrylate
  • AETAC copolymer of acrylamide and acrylamidopropyl trimethyl ammonium chloride
  • AETAC copolymer of acrylamide and acryloloxyethyl trimethyl ammonium chloride
  • the anionic synthetic polymers are formed from one or more ethylenically unsaturated anionic monomers or a blend of one or more anionic monomers with one or more of the nonionic monomers mentioned previously.
  • the anionic monomers include acrylic acid, methacrylic acid, maleic acid, crotonic acid, itaconic acid, vinyl suifonic acid, allyl suifonic acid, 2-acrylamido-2- methylpropane sulfonic acid (AMPS), acrylamide, mixtures thereof, and salts thereof.
  • copolymers and/or terpolymers of monomers selected from the group consisting of acrylamide, AMPS, acrylic acid, and (meth)acrylic acid are copolymers and/or terpolymers of monomers selected from the group consisting of acrylamide, AMPS, acrylic acid, and (meth)acrylic acid.
  • the anionic polymer may be selected from the group consisting of copolymers derived from 2-acrylamido 2-methyipropane suifonic acid, copolymers of acrylic acid and acrylamide, homopolymers of acrylic acid, homopolymers of acrylamide, and combinations thereof.
  • anionic polymer are the copolymer of sodium acrylate and acrylamide and the copolymer of acrylic acid and acrylamide.
  • copolymers of AMPS and acrylamide wherein the mole percent of AMPS is from about 10 mole percent to about 25 mole percent
  • terpolymers of AMPS, acrylamide, and acrylic acid wherein the mole percent of AMPS is from about 10 mole percent to about 30 mole percent
  • the mole percent of acrylamide is from about 40 mole percent to about 60 mole percent
  • the mole percent of acrylic acid is from about 20 mole percent to about 40 mole percent.
  • homopolymers of acrylic acid or copolymers of acrylic acid and acrylamide are of particular interest.
  • the filtration aid promoter and synthetic polymer are applied in methods for separating solids from a liquid dispersion.
  • This process comprises the steps of adding the filtration aid promoter and synthetic polymer to an aqueous dispersion of solids in liquids prior to and/or during the physical separation of the solids from the liquid resulting in a concentrate comprising solids, recovering the concentrate and then filtering the concentrate.
  • Enhanced filtration is achieved with this method.
  • Physical separation can occur by allowing the solids to settle from the liquid through force of gravity, optionally with flocculation and/or agglomeration of the solid particles.
  • the method may be applied in mining operations.
  • a method for dewatering mining slurries, in particular enhanced filtration performance, in a two step process having a liquid solid separation step and a filtration step comprises adding at least one filtration aid promoter and at least one synthetic polymer to the mining slurry during or before, or both during and before, the liquid solid separation step and then filtering the concentrate or underflow from the liquid solid separation step.
  • the mining slurries are aqueous dispersions comprising minerals, such as those selected from the group consisting of gold, phosphate, silver, platinum, copper, nickel, zinc, lead, molybdenum, iron, coal and the like.
  • the liquid solid separation step is performed in a means for separating liquids from solids, such as a gravity thickener, clarifier or hydrocyclone and the filtration aid promoter and synthetic polymer may be added to the aqueous dispersion while the dispersion is in such means and/or prior to the dispersion entering such means.
  • the filtration step is generally conducted in a means for filtering solids from liquids, such as a filter press or vacuum filter.
  • aqueous dispersion samples were prepared by adding 1000 mL of an aqueous dispersion to a graduated cylinder, where it was treated by adding the specified components of the filtration aid promoter (i.e. coagulant, natural polymer and/or semi-natural polymer) as set forth in Table I, and tamping the filtration aid promoter into the dispersion three times with a plunger having perforated holes.
  • the filtration aid promoter i.e. coagulant, natural polymer and/or semi-natural polymer
  • Synthetic Polymer A used in the Examples is an anionic copolymer available under the trade name FLOPA ® AN 1 13 from SNF Floerger, Andrezieu, France.
  • the suppliers and/or trade names for the synthetic polymer and the component(s) of the filtration aid promoter are set forth in Table IA.
  • filtration rates were then calculated and compared to the corresponding comparative example to provide a percentage measure of the increase in filtration rate (% 10 mLs and % 20 mLs). These values and the average of % 10 mLs and % 20 mLs are set forth in Table II.
  • the natural and semi-natural polymers used and the ratio of natural and semi-natural polymers to Synthetic Polymer A are set forth in Table IV.
  • the times for filtering 30 and 60 mL were measured.
  • the filtration rates were then calculated and compared to the corresponding comparative example to provide a percentage measure of the increase in filtration rate ⁇ % 30 ml_s and % 60 mLs).
  • These values and the average of % 30 mLs and % 60 mLs are set forth in Table IV.
  • the dosage of flocculant (Synthetic Polymer A) in the examples was 144.1 grams per ton, while the ratio of natural or semi-natural polymers with coagulant to synthetic polymer varied from 0 to 100%.
  • the natural or semi- natural polymers with coagulant used and the ratio of such natural or semi- natural polymers with coagulant to Synthetic Polymer A are set forth in Table V.
  • the times for filtering 30 and 60 mL were measured.
  • the filtration rates were then calculated and compared to the corresponding comparative example to provide a percentage measure of the increase in filtration rate (% 30 mLs and % 60 mLs). These values and the average of % 30 mLs and % 60 mLs are set forth in Table V.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)
  • Treatment Of Sludge (AREA)
PCT/US2013/059694 2012-09-19 2013-09-13 Process for filtration enhancement of aqueous dispersions WO2014046979A1 (en)

Priority Applications (7)

Application Number Priority Date Filing Date Title
EP13839337.6A EP2897707A4 (en) 2012-09-19 2013-09-13 METHOD FOR IMPROVING FILTRATION OF AQUEOUS DISPERSIONS
AU2013318334A AU2013318334B2 (en) 2012-09-19 2013-09-13 Process for filtration enhancement of aqueous dispersions
CN201380048874.8A CN104640612A (zh) 2012-09-19 2013-09-13 增强含水分散体的过滤的方法
CA2883633A CA2883633C (en) 2012-09-19 2013-09-13 Process for filtration enhancement of aqueous dispersions
BR112015005846-9A BR112015005846B1 (pt) 2012-09-19 2013-09-13 Método e composição para melhorar a filtração de suspensões minerais
MX2015003298A MX2015003298A (es) 2012-09-19 2013-09-13 Proceso para mejorar la filtracion de dispersiones acuosas.
ZA2015/02608A ZA201502608B (en) 2012-09-19 2015-04-17 Process for filtration enhancement of aqueous dispersions

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US201261702774P 2012-09-19 2012-09-19
US61/702,774 2012-09-19

Publications (1)

Publication Number Publication Date
WO2014046979A1 true WO2014046979A1 (en) 2014-03-27

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ID=50341874

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/US2013/059694 WO2014046979A1 (en) 2012-09-19 2013-09-13 Process for filtration enhancement of aqueous dispersions

Country Status (10)

Country Link
EP (1) EP2897707A4 (es)
CN (1) CN104640612A (es)
AU (1) AU2013318334B2 (es)
BR (1) BR112015005846B1 (es)
CA (1) CA2883633C (es)
CL (1) CL2015000672A1 (es)
MX (1) MX2015003298A (es)
PE (1) PE20150931A1 (es)
WO (1) WO2014046979A1 (es)
ZA (1) ZA201502608B (es)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017182568A1 (en) 2016-04-21 2017-10-26 Basf Se Amphoteric polymer, process for production thereof, and use thereof, to treat aqueous dispersions
CN113461928A (zh) * 2021-06-30 2021-10-01 上海抚佳精细化工有限公司 一种低凝点聚醚及其组合物和其制备方法和应用

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106215893A (zh) * 2016-08-17 2016-12-14 鞍钢集团矿业有限公司 一种低品位铁矿粉的助滤剂

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US3171802A (en) * 1962-11-14 1965-03-02 Gen Services Company Sewage treatment
US5904853A (en) * 1996-11-26 1999-05-18 Microbar Incorporated Wastewater treatment process and apparatus for high flow silica removal
US20110233124A1 (en) * 2008-10-15 2011-09-29 Pentti Virtanen Acidic water and its use for drainage or separation of solids

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CA914925A (en) * 1972-11-21 Simonacco Limited Process for the concentration of the solid content of aqueous suspensions containing clay minerals
US3541009A (en) * 1968-12-18 1970-11-17 Nalco Chemical Co Polymer-polysaccharide-caustic alkali compositions and process of separating solids from aqueous suspensions therewith
CA2248479A1 (en) * 1997-09-29 1999-03-29 Calvin T. Tobison Starch/cationic polymer combinations as coagulants for the mining industry
GB0029077D0 (en) * 2000-11-29 2001-01-10 Ciba Spec Chem Water Treat Ltd Flocculation of mineral suspensions
GB0405505D0 (en) * 2004-03-12 2004-04-21 Ciba Spec Chem Water Treat Ltd Dewatering process
GB0405506D0 (en) * 2004-03-12 2004-04-21 Ciba Spec Chem Water Treat Ltd Dewatering process

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
US3171802A (en) * 1962-11-14 1965-03-02 Gen Services Company Sewage treatment
US5904853A (en) * 1996-11-26 1999-05-18 Microbar Incorporated Wastewater treatment process and apparatus for high flow silica removal
US20110233124A1 (en) * 2008-10-15 2011-09-29 Pentti Virtanen Acidic water and its use for drainage or separation of solids

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of EP2897707A4 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017182568A1 (en) 2016-04-21 2017-10-26 Basf Se Amphoteric polymer, process for production thereof, and use thereof, to treat aqueous dispersions
CN113461928A (zh) * 2021-06-30 2021-10-01 上海抚佳精细化工有限公司 一种低凝点聚醚及其组合物和其制备方法和应用

Also Published As

Publication number Publication date
BR112015005846B1 (pt) 2021-06-22
AU2013318334A1 (en) 2015-03-05
CN104640612A (zh) 2015-05-20
PE20150931A1 (es) 2015-06-10
ZA201502608B (en) 2017-09-27
EP2897707A4 (en) 2016-10-26
BR112015005846A2 (pt) 2017-07-04
CL2015000672A1 (es) 2015-08-07
CA2883633C (en) 2017-04-11
EP2897707A1 (en) 2015-07-29
AU2013318334B2 (en) 2016-06-09
CA2883633A1 (en) 2014-03-27
MX2015003298A (es) 2015-07-14

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