NO327217B1 - Polyaluminum nitrate sulfates, their preparation and use - Google Patents
Polyaluminum nitrate sulfates, their preparation and use Download PDFInfo
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- NO327217B1 NO327217B1 NO20006218A NO20006218A NO327217B1 NO 327217 B1 NO327217 B1 NO 327217B1 NO 20006218 A NO20006218 A NO 20006218A NO 20006218 A NO20006218 A NO 20006218A NO 327217 B1 NO327217 B1 NO 327217B1
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- nitrate
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- aluminum
- polyaluminium
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- ZODDGFAZWTZOSI-UHFFFAOYSA-N nitric acid;sulfuric acid Chemical class O[N+]([O-])=O.OS(O)(=O)=O ZODDGFAZWTZOSI-UHFFFAOYSA-N 0.000 title claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 22
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 21
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 10
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 9
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 8
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000011575 calcium Substances 0.000 claims abstract description 4
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 4
- 238000005189 flocculation Methods 0.000 claims description 10
- -1 polydadmac Polymers 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- 230000016615 flocculation Effects 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 230000029087 digestion Effects 0.000 claims description 8
- 230000002452 interceptive effect Effects 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 239000004411 aluminium Substances 0.000 claims description 6
- 239000003651 drinking water Substances 0.000 claims description 6
- 235000020188 drinking water Nutrition 0.000 claims description 6
- 230000014759 maintenance of location Effects 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 229920000867 polyelectrolyte Polymers 0.000 claims description 6
- 238000004062 sedimentation Methods 0.000 claims description 6
- 238000004026 adhesive bonding Methods 0.000 claims description 5
- 239000010440 gypsum Substances 0.000 claims description 5
- 229910052602 gypsum Inorganic materials 0.000 claims description 5
- 229920002472 Starch Polymers 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 229920002401 polyacrylamide Polymers 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 239000008107 starch Substances 0.000 claims description 4
- 235000019698 starch Nutrition 0.000 claims description 4
- 229920000768 polyamine Polymers 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 230000009182 swimming Effects 0.000 claims description 2
- 239000002699 waste material Substances 0.000 claims description 2
- 230000003472 neutralizing effect Effects 0.000 abstract description 2
- 229910052925 anhydrite Inorganic materials 0.000 abstract 1
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 abstract 1
- 235000011149 sulphuric acid Nutrition 0.000 abstract 1
- 150000001805 chlorine compounds Chemical class 0.000 description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 5
- 239000008394 flocculating agent Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- FZUJWWOKDIGOKH-UHFFFAOYSA-N sulfuric acid hydrochloride Chemical class Cl.OS(O)(=O)=O FZUJWWOKDIGOKH-UHFFFAOYSA-N 0.000 description 3
- 229910021653 sulphate ion Inorganic materials 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- CSDQQAQKBAQLLE-UHFFFAOYSA-N 4-(4-chlorophenyl)-4,5,6,7-tetrahydrothieno[3,2-c]pyridine Chemical compound C1=CC(Cl)=CC=C1C1C(C=CS2)=C2CCN1 CSDQQAQKBAQLLE-UHFFFAOYSA-N 0.000 description 1
- 229910018626 Al(OH) Inorganic materials 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- BUACSMWVFUNQET-UHFFFAOYSA-H dialuminum;trisulfate;hydrate Chemical compound O.[Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BUACSMWVFUNQET-UHFFFAOYSA-H 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000504 effect on taste Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 150000002506 iron compounds Chemical class 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical class Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- 159000000014 iron salts Chemical class 0.000 description 1
- 229910000358 iron sulfate Inorganic materials 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- DNHVXYDGZKWYNU-UHFFFAOYSA-N lead;hydrate Chemical compound O.[Pb] DNHVXYDGZKWYNU-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000011505 plaster Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
Classifications
-
- 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
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/78—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
- C01F7/786—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen containing, besides aluminium, only anions, e.g. Al[OH]xCly[SO4]z
-
- 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
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment 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
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/66—Salts, e.g. alums
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/26—Nature of the water, waste water, sewage or sludge to be treated from the processing of plants or parts thereof
- C02F2103/28—Nature of the water, waste water, sewage or sludge to be treated from the processing of plants or parts thereof from the paper or cellulose industry
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/42—Nature of the water, waste water, sewage or sludge to be treated from bathing facilities, e.g. swimming pools
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/02—Agents for preventing deposition on the paper mill equipment, e.g. pitch or slime control
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/06—Paper forming aids
- D21H21/10—Retention agents or drainage improvers
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
- D21H21/16—Sizing or water-repelling agents
Abstract
Description
Foreliggende oppfinnelse angår polyaluminiumnitratsulfater, deres fremstilling og anvendelse. The present invention relates to polyaluminium nitrate sulphates, their production and use.
Ved vannopparbeiding anvender man vanligvis som flokkulerings- og koaguleringsmiddel, avhengig av type og tilsmusning, aluminiumforbindelser som aluminiumklorid, aluminiumsulfat, polyaluminiumklorider, jernforbindelser som jernsulfat eller jernklorider, samt kationiske, anioniske og ikke-ioniske polyelektrolytter som polyakrylamid, polydadmac, polyamin og sjiktsilikater som bentonitt. In water treatment, aluminum compounds such as aluminum chloride, aluminum sulfate, polyaluminium chlorides, iron compounds such as iron sulfate or iron chlorides, as well as cationic, anionic and non-ionic polyelectrolytes such as polyacrylamide, polydadmac, polyamine and layer silicates such as bentonite are usually used as flocculating and coagulant agents, depending on the type and soiling. .
Ved siden av disse tradisjonelt anvendte produkter anvendes det i de senere år i økende grad aluminiumhydroksydklorider som flokkuleringsmidler, særlig for kompliserte oppgaver, for eksempel på drikkevannsområdet. Alumiumhydroksydklorider er kjent som polyaluminiumklorider (PAC) og karakteriseres ved formelen [Al(OH)x Cly]n, x+y = 3. Derfor er n et med en polymeriseringsgrad sammenlignbart antall aluminiumioner i aluminiumkomplekset. Polymere aluminiumhydroksydklorider egner seg bedre for flokkulering og koagulering enn de enkle aluminiumsalter hvorigjennom de nødvendige doseringsmengder kan reduseres. Brukserfaringer viser en forbedret blakkingsmaterialaggregering slik at man delvis kan gi avkall på tilsetning av flokkuleringshjelpemidler. Anvendelsen av polyaluminiumklorider bevirker i tillegg en mindre reduksjon av pH-verdiene og i tillegg er innføringen av anioner i vannet mindre enn ved anvendelse av nøytralsalter. Til slutt kan nevnes en bedre virksomhet av polyaluminiumklorider ved lavere vanntemperaturer, noe som er av uvurderlig fordel ved vinterdrift. In addition to these traditionally used products, in recent years aluminum hydroxide chlorides are increasingly being used as flocculating agents, particularly for complicated tasks, for example in the area of drinking water. Aluminum hydroxide chlorides are known as polyaluminum chlorides (PAC) and are characterized by the formula [Al(OH)x Cly]n, x+y = 3. Therefore, n is a number of aluminum ions in the aluminum complex comparable to a degree of polymerization. Polymeric aluminum hydroxide chlorides are better suited for flocculation and coagulation than the simple aluminum salts, through which the required dosage amounts can be reduced. Experience shows an improved flocculation material aggregation so that the addition of flocculation aids can be partially dispensed with. The use of polyaluminium chlorides also causes a smaller reduction in the pH values and, in addition, the introduction of anions into the water is less than when neutral salts are used. Finally, mention can be made of the better activity of polyaluminium chlorides at lower water temperatures, which is of inestimable advantage in winter operation.
Alle flokkuleirngsmidler må fjernes fra vannet igjen ved flokkuleringsprosessen og kan ikke overskride lovmessig fastlagte grenseverdier. Polyelektrolyttrester i drikkevannet er i mange tilfeller en sunnhetsrisiko på grunn av restmonomeirnnholdet. Jernsalter som er tilbake i vannet fører til en gulfarging og når det gjelder drikkevannet også til en smakspåvirkning. Jern- og aluminiumkonsentrasjoner er i drikkevanns- som i avfallsvannområdet bundet av et strengt regelverk. All flocculants must be removed from the water again during the flocculation process and cannot exceed legally established limit values. Polyelectrolyte residues in the drinking water are in many cases a health risk due to the residual monomer content. Iron salts that are back in the water lead to a yellow color and, in the case of drinking water, also to an effect on taste. Iron and aluminum concentrations in drinking water and in the waste water area are bound by strict regulations.
I papirindustrien anvendes polyaluminiumklorider for fiksering av forstyrrende stoffer, liming, retensjon, awanning, stivelsesfiksering og avfallsvannoptimering. Fordelen ved polyaluminiumklorider i forhold til aluminiumsulfat ligger i en lavere systemoppsalting, en lavere pH-verdisenking, en bedre fiksering av forstyrrelses-, fin- og hjelpestoffer og den ulike lavere krittoppløsning ved nøytraldirftsmodus. In the paper industry, polyaluminium chlorides are used for the fixation of interfering substances, gluing, retention, dewatering, starch fixation and waste water optimization. The advantage of polyaluminium chlorides compared to aluminum sulphate lies in a lower system salinization, a lower pH value reduction, a better fixation of disturbing, fine and auxiliary substances and the various lower chalk dissolution in neutral soil mode.
Polyaluminiumklorider henholdsvis polyaluminiumkloridsulfater fremstilles som regel i henhold til to metoder. For det første oppsluttes et aluminiumholdig råstoff som alumimumhydroksid med svovelsyre og saltsyre og nøytraliseres med en basisk, kalsiumholdig reagens som for eksempel kalsiumklorid eller kalsiumhydrid. Den her oppnådde gips separeres (DE-A-1907359, US-A-5603912, US-A-5124139). For det andre oppsluttes et aluminiumholdig råstoff som aluminiumhydroksyd i overskudd med svovelsyre og saltsyre i en trykkreaktor ved temperaturer over 130°C. Den oppnådde oppslutningsrest er som regel ikke stabil og må fortynnes med vann (DE-A-2163711, EP-A-0884278). Ved den tiltagende omstilling til lukket vannkretsløp i industrien opptrer ved anvendelse av kloridholdige prosesskjemikalier i disse systemer relativt høye kloridkonsentrasjoner på opp til 3.000 mg/l. Disse kloridkonsentrasjoner kan føre til betydelige korrosjonsfenomener på deler i anleggene. Anvendelsen av polyaluminiumklorider bidrar likeledes til å forhøye kloridtransporten. Polyaluminium chlorides or polyaluminium chloride sulphates are usually produced according to two methods. Firstly, an aluminum-containing raw material such as aluminum hydroxide is digested with sulfuric acid and hydrochloric acid and neutralized with a basic, calcium-containing reagent such as calcium chloride or calcium hydride. The gypsum obtained here is separated (DE-A-1907359, US-A-5603912, US-A-5124139). Secondly, an aluminium-containing raw material such as aluminum hydroxide is digested in excess with sulfuric acid and hydrochloric acid in a pressure reactor at temperatures above 130°C. The digestion residue obtained is usually not stable and must be diluted with water (DE-A-2163711, EP-A-0884278). With the increasing conversion to a closed water circuit in industry, the use of chloride-containing process chemicals in these systems results in relatively high chloride concentrations of up to 3,000 mg/l. These chloride concentrations can lead to significant corrosion phenomena on parts of the facilities. The use of polyaluminium chlorides also contributes to increasing chloride transport.
Oppgave for foreliggende oppfinnelse er å tilveiebringe et flokkuleirngsmiddel for vannbehandling der de ovenfor angitte mangler kan unngås, som danner kompakte, stabile, ved flotering eller sedimentering lett fjernbare fnokker fra vannet og som er egnet i papirindustrien for fiksering av forstyrrende stoffer, liming, retensjon, awanning og stivelsesfiksering. The task of the present invention is to provide a flocculant for water treatment where the above-mentioned shortcomings can be avoided, which forms compact, stable, easily removable flocs from the water by flotation or sedimentation and which is suitable in the paper industry for fixing interfering substances, gluing, retention, dewatering and starch fixation.
Denne oppgave løses ved polyaluminiumnitratsulfater med sammensetningen: This task is solved by polyaluminium nitrate sulphates with the composition:
5,0 til 5,6 vekt-% aluminium 5.0 to 5.6% aluminum by weight
2,4 til 3,25 vekt-% sulfat 2.4 to 3.25% by weight sulfate
14,5 til 24,0 vekt-% nitrat, 14.5 to 24.0% by weight nitrate,
hvorved resten til 100 vekt-% er vann. whereby the remainder to 100% by weight is water.
Ved tilsetning av polyelektrolytter som polyakrylamid, polydadmac, polyamin osv., oppnår man innenfor rammen av den fordelaktige utførelsesform av oppfinnelsen en utmerket flokkulering og koagulering. By adding polyelectrolytes such as polyacrylamide, polydadmac, polyamine, etc., excellent flocculation and coagulation is achieved within the framework of the advantageous embodiment of the invention.
Polyaluminiumnitratsulfatene fremstilles ved at aluminiumholdig råstoff som aluminiumhydroksyd, bauxitt, aluminiumholdige filterslam osv. støkiometrisk oppsluttes med en blanding av svovel- og salpetersyre ved temperaturer fra 50 til 130°C, nøytraliserer oppslutningsresten med basiske kalsiumholdig reagens som kalsiumkarbonat eller kalsiumhydroksyd og separerer den dannede gips. The polyaluminium nitrate sulfates are produced by stoichiometrically digesting aluminum-containing raw material such as aluminum hydroxide, bauxite, aluminum-containing filter sludge, etc. with a mixture of sulfuric and nitric acid at temperatures from 50 to 130°C, neutralizing the digestion residue with basic calcium-containing reagents such as calcium carbonate or calcium hydroxide and separating the gypsum formed.
Hensiktsmessig filtreres gipsen fra ved temperaturer fra 60 til 70°C og vaskes. Appropriately, the plaster is filtered off at temperatures from 60 to 70°C and washed.
Den nøytraliserte oppslutningsrest fortynnes i forhold 1,5:1 til 2,5:1, hvorved det som fortynningsmiddel fortrinnsvis anvendes vaskefiltrat. The neutralized digestion residue is diluted in a ratio of 1.5:1 to 2.5:1, whereby washing filtrate is preferably used as diluent.
Alternativt foreligger det en mulighet for å slutte opp det aluminiumholdige råstoff på understøkiometrisk måte med en blanding av svovel- og salpetersyre under et trykk på 1,0 til 3,0 bar ved temperaturer fra 130 til 200°C og så separerer uoppløselige bestanddeler. Alternatively, there is a possibility to substoichiometrically digest the aluminium-containing raw material with a mixture of sulfuric and nitric acid under a pressure of 1.0 to 3.0 bar at temperatures from 130 to 200°C and then separate insoluble components.
Da denne oppslutningsrest som regel ikke er stabil, skjer det en fortynning med vann i forholdet 0,6:1 til 2:1. Ved anvendelse av aluminiumsulfat som aluminiumholdig råstoff er det tilstrekkelig når oppslutningen gjennomføres med salpetersyre. As this digestion residue is usually not stable, it is diluted with water in a ratio of 0.6:1 to 2:1. When aluminum sulfate is used as an aluminum-containing raw material, it is sufficient when digestion is carried out with nitric acid.
Oppfinnelsen angår videre anvendelse av polyaluminiumnitratsilikater fremstilt ifølge oppfinnelsen som flokkulerings- og sedimenteringsmiddel for drikkevanns-, svømmebassengvanns- og avfallsopparbeiding og som hjelpemiddel for papirfremstilling for liming, fiksering av forstyrrende stoffer, awanning, stivelsesfiksering og retensjon. The invention further relates to the use of polyaluminium nitrate silicates produced according to the invention as a flocculation and sedimentation agent for drinking water, swimming pool water and waste treatment and as an aid for paper production for gluing, fixation of interfering substances, dewatering, starch fixation and retention.
Oppfinnelsen skal forklares nærmere ved hjelp av de følgende illustrerende utførelseseksempler: The invention shall be explained in more detail by means of the following illustrative examples:
1. Første utførelseseksempel: 1. First embodiment example:
200 g aluminiumhydroksyd oppløses i 246 g svovelsyre (78%) og 268,2 g salpetersyre (65%) i en 2 1 glassbeholder under omrøring ved en temperatur av 80°C i løpet av 40 minutter og det dannede konsentrat fortynnes med 200 ml vann. I denne oppløsning røres det inn en suspensjon av 175 g kalsiumkarbonat og 175 g vann rundt 60°C. Den dannede gips filtreres av ved 63°C og vaskes og det nøytraliserte konsentratet fortynnes med vaskefiltrat i forholdet 2:1. Det oppnådde polyaluminiumnitratsulfatet består av 5,3 vekt-% aluminium, 2,7 vekt-% sulfat og 18,2 vekt-% nitrat. 200 g of aluminum hydroxide is dissolved in 246 g of sulfuric acid (78%) and 268.2 g of nitric acid (65%) in a 2 1 glass container with stirring at a temperature of 80°C during 40 minutes and the resulting concentrate is diluted with 200 ml of water . A suspension of 175 g of calcium carbonate and 175 g of water at around 60°C is stirred into this solution. The gypsum formed is filtered off at 63°C and washed and the neutralized concentrate is diluted with washing filtrate in a ratio of 2:1. The obtained polyaluminium nitrate sulphate consists of 5.3% by weight aluminium, 2.7% by weight sulphate and 18.2% by weight nitrate.
2. Utførelseseksempel: 2. Execution example:
270 g aluminiumhydroksyd i 67,6 g svovelsyre (78%) og 428,8 g salpetersyre (65%) oppsluttes i en trykkréaktor ved 2,5 bar under omrøring ved en temperatur av 150°C i løpet av 60 minutter. De uoppløselige bestanddeler filtreres av og konsentratet fortynnes med vann i forholdet 2:1. Det oppnådde polyaluminiumnitratsulfat består av 5,3 vekt-% aluminium, 2,5 vekt-% sulfat og 17,8 vekt-% nitrat. 270 g of aluminum hydroxide in 67.6 g of sulfuric acid (78%) and 428.8 g of nitric acid (65%) are dissolved in a pressure reactor at 2.5 bar with stirring at a temperature of 150°C during 60 minutes. The insoluble components are filtered off and the concentrate is diluted with water in a ratio of 2:1. The obtained polyaluminium nitrate sulphate consists of 5.3% by weight aluminium, 2.5% by weight sulphate and 17.8% by weight nitrate.
3. Utførelseseksempel: 3. Execution example:
Det i henhold til 1. utførelseseksempel fremstilte polyaluminiumnitratsulfat blandes med en flytende polyelektrolytt på basis av et polyakrylamid i forholdet 9:1. Det på denne måte oppnådde produkt består av 4,8 vekt-% aluminium, 2,4 vekt-% sulfat, 16,4 vekt-% nitrat og 1,2 vekt-% polyelektrolytt. The polyaluminium nitrate sulfate produced according to the 1st embodiment is mixed with a liquid polyelectrolyte based on a polyacrylamide in a ratio of 9:1. The product obtained in this way consists of 4.8% by weight aluminium, 2.4% by weight sulphate, 16.4% by weight nitrate and 1.2% by weight polyelectrolyte.
4. Utførelseseksempel: 4. Execution example:
Man sammenligner de i henhold til utførelseseksemplene 1 til 3 fremstilte polyaluminiumnitratsulfater med et konvensjonelt polyaluminiumkloridsulfat som er fremstilt i henhold til DE-A-1907359 når det gjelder flokkuleringsoppførselen. For dette formål anvendes en Jar-test med et vann som er kunstig tilsmusset med 100 ppm pulverformig aktivkull. Den doserte aluminiumkonsentrasjonen utgjør 5,3 ppm. The polyaluminium nitrate sulfates produced according to embodiments 1 to 3 are compared with a conventional polyaluminum chloride sulfate produced according to DE-A-1907359 with regard to the flocculation behavior. For this purpose, a Jar test is used with water artificially contaminated with 100 ppm powdered activated carbon. The dosed aluminum concentration amounts to 5.3 ppm.
For prøving av flokkuleringsvirkningen av primærflokkuleringsmidler gjennomføres For testing the flocculation effect of primary flocculants is carried out
begerglassforsøk eller Jar-test. For i størst mulig grad å utelukke forskjellige mekaniske innflytelser gjennomføres sammenlignende flokkuleringsprøver i en serie av begerglass med mekanisk koblede og identisk tildannede bladrørere, hvorved produktene som skal sammenlignes settes til samtidig. For nøyaktig dosering tilsettes flokkuleringsmidlene som skal utprøves som 10%-ig oppløsning. Etter å ha satt til 11 vann pr. begerglass, blandes det kort inn 1,0 ml aktivkullsuspensjon under omrøring. Det således kunstig tilsmussede vann prøves på pH-verdi, temperatur og eventuelt på alkali-Zjordalkali-innhold. Etter tilmåling av en aluminiumlik doseringsmengde settes denne doseringsmengde samtidig til de enkelte testmønstre og blandes inn under sterk omrøring (200 til 220 opm) i 60 sekunder. Deretter røres det i 4 minutter ved 20 til 30 opm. Etter å ha trukket ut rørebladene skal de dannede fnokker sedimentere i ca. 25 minutter. Parametrenes fnokkdannelse, fhokkstørrelse, sedimenterings- og blakkingstoffelimineringshastighet bestemmer sammen virkningen av et flokkuleringsmiddel. Allerede under innblandings- og etterrøringsfasen kan man observere visuelt den pågående mokkdannelse samt utviklingen av fhokkstørrelsen for de angjeldende produkter med tiden og beskrive disse relativt hverandre. Videre fastholdes sedimentasjonsoppførselen for fnokkene og videre kontrolleres pH-verdi og beaker test or Jar test. In order to rule out different mechanical influences to the greatest extent possible, comparative flocculation tests are carried out in a series of beakers with mechanically linked and identically designed blade stirrers, whereby the products to be compared are added at the same time. For accurate dosage, the flocculating agents to be tested are added as a 10% solution. After adding 11 water per beaker, briefly mix in 1.0 ml of activated charcoal suspension while stirring. The thus artificially polluted water is tested for pH value, temperature and possibly for alkali-Zjordalkali content. After measuring a dosage amount similar to aluminum, this dosage amount is added to the individual test patterns at the same time and mixed in under vigorous stirring (200 to 220 rpm) for 60 seconds. It is then stirred for 4 minutes at 20 to 30 rpm. After pulling out the stir-fry leaves, the formed clumps should settle for approx. 25 minutes. The parameters floc formation, floc size, sedimentation and flocculant elimination rate together determine the effectiveness of a flocculant. Already during the mixing and post-stirring phase, you can visually observe the ongoing muck formation as well as the development of the muck size for the products in question over time and describe these relative to each other. Furthermore, the sedimentation behavior of the floes is maintained and the pH value and
temperatur. Klarheten i supernatanten bestemmes ved blakkingsmåling etter sedimentering. For dette formål fjernes 50 til 75 ml av supernatanten fra midlere begerglasshøyde og blakkingen angis i formazien-nefelometrienheter. Forsøksresultatene er oppsummert i tabell 1. temperature. The clarity of the supernatant is determined by clouding measurement after sedimentation. For this purpose, 50 to 75 ml of the supernatant is removed from the mean beaker height and the dilution is indicated in formazin nephelometric units. The test results are summarized in table 1.
Resultatene av Jar-testen viser at produktene i henhold til anvendelseseksemplene 1-3 er likeverdige med en PAC i henhold til DE 1907359, og når det gjelder fnokkstørrelse sågar overlegen. The results of the Jar test show that the products according to application examples 1-3 are equivalent to a PAC according to DE 1907359, and in terms of fluff size even superior.
5. Utførelseseksempel: 5. Execution example:
De ifølge utførelseseksemplene 1 til 3 fremstilte polyaluminiumnitratsulfater sammenlignes i en papirfremstillingsprosess med et konvensjonelt polyaluminiumkloridsulfat, fremstilt i henhold til metoden ifølge DE-A-1907359, når det gjelder awanningsoppførsel, ved fiksering av forstyrrende stoffer samt ved liming. Awanningsforsøkene gjennomføres på et Schopper-Riegler-apparat (i henhold til datablad V/7/61 fra "Vereins der Zellstoff- und Papirchemiker und -ingenieure). Man måler awanningstiden for en standardmasse av 70% cellulose og 30% gammelt papir. Restblakkingen for filtratet og det kjemiske oksygenbehov (COD), gir opplysninger om retensjonen og fikseringen av forstyrrende stoffer for polyaluminiumnitratsulfatene. Limingen testes på en standardpapirsystem (2,4 g atomsfæretørket cellulose, prøveblad 80 g/m<2>,20% CaCCh) med forskjellige limkonsentrasjoner over Cobbeo i henhold til DIN 53 132. The polyaluminium nitrate sulfates produced according to embodiments 1 to 3 are compared in a papermaking process with a conventional polyaluminium chloride sulfate, produced according to the method according to DE-A-1907359, in terms of dewatering behavior, when fixing interfering substances and when gluing. The dewatering experiments are carried out on a Schopper-Riegler apparatus (according to data sheet V/7/61 from "Vereins der Zellstoff- und Papirchemiker und -ingeniure). The dewatering time is measured for a standard mass of 70% cellulose and 30% old paper. The residual blackening for the filtrate and the chemical oxygen demand (COD), provide information on the retention and fixation of interfering substances for the polyaluminium nitrate sulfates.The bonding is tested on a standard paper system (2.4 g atomized cellulose, sample sheet 80 g/m<2>,20% CaCCh) with different glue concentrations over Cobbeo according to DIN 53 132.
Tabell 2 viser klart at alle typer polyaluminiumnitratsulfat oppfører seg som konvensjonelle polyaluminiumklorider ved papiranvendelse både når det gjelder awanningsoppførsel, ved retensjon og fiksering av forstyrrende stoffer. For alle polyaluminiumnitratsulfater oppnås noe høyere Cobbgo-verdier enn ved et sammenlignbart polyaluminiumklorid. Limingsoppførselen er derved noe svakere enn ved de konvensjonelle polyaluminiumklorider. Table 2 clearly shows that all types of polyaluminium nitrate sulphate behave like conventional polyaluminium chlorides when used in paper, both in terms of dewatering behaviour, retention and fixation of interfering substances. For all polyaluminium nitrate sulphates somewhat higher Cobbgo values are obtained than with a comparable polyaluminium chloride. The bonding behavior is therefore somewhat weaker than with the conventional polyaluminium chlorides.
De med oppfinnelsen oppnådde fordeler ligger særlig i at det ved samme oppnådde virkning for polyaluminiumnitratsulfatene sammenlignet med polyaluminiumklorid, The advantages achieved with the invention lie in particular in that, with the same effect achieved for the polyaluminium nitrate sulphates compared to polyaluminium chloride,
ikke lenger innføres klorid i lukkede vannkretsløp. Herved kan man, særlig ved anvendelse ved papirfremstilling eller i lukkede papirkretsløp, betydelig senke chloride is no longer introduced into closed water circuits. In this way, particularly when used in paper production or in closed paper circuits, it can be significantly reduced
korrosjonspotentialet for vannberørte ståldeler og som oppstår ved oppkonsentrering av klorid. the corrosion potential for steel parts in contact with water and which occurs when chloride is concentrated.
Claims (8)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19960702 | 1999-12-16 |
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| NO20006218D0 NO20006218D0 (en) | 2000-12-07 |
| NO20006218L NO20006218L (en) | 2001-06-18 |
| NO327217B1 true NO327217B1 (en) | 2009-05-11 |
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| EP (1) | EP1108679B1 (en) |
| AT (1) | ATE251598T1 (en) |
| DE (1) | DE50003987D1 (en) |
| DK (1) | DK1108679T3 (en) |
| ES (1) | ES2208207T3 (en) |
| NO (1) | NO327217B1 (en) |
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| DE10147658A1 (en) * | 2001-09-27 | 2003-04-10 | Cu Chemie Uetikon Ag Uetikon | Composition and its use as a coagulant and flocculant |
| RU2007142564A (en) * | 2005-04-21 | 2009-05-27 | Захтлебен Шеми ГмбХ (DE) | MEANS FOR USE IN WATER TREATMENT |
| WO2008090231A2 (en) * | 2007-01-26 | 2008-07-31 | Sachtleben Chemie Gmbh | Method for preventing unwanted formation of hydrogen sulfide during the isolation of biogas by the addition of nitrate salts |
| FI129034B (en) * | 2019-06-14 | 2021-05-31 | Kemira Oyj | Use of a treatment system comprising wood-based organic material for removing dissolved organic compounds from wastewater |
| CN112142085A (en) * | 2020-08-04 | 2020-12-29 | 广西锋华环保科技有限公司 | Method for producing polyaluminum sulfate by using aluminum ash |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| GB950208A (en) * | 1961-05-09 | 1964-02-19 | Albright & Wilson Mfg Ltd | Basic aluminium salts |
| DE1907359B2 (en) * | 1969-02-14 | 1978-09-14 | Taki Fertilizer Manufacturing Co., Ltd., Kakogawa (Japan) | Flocculant solutions and processes for their preparation |
| DE3675140D1 (en) * | 1985-07-12 | 1990-11-29 | Rhone Poulenc Chimie | BASIC ALUMINUM CHLORINE SULFATE, METHOD FOR THE PRODUCTION THEREOF AND ITS USE AS A COAGULATING AGENT. |
| IT1229503B (en) * | 1989-01-25 | 1991-09-03 | Caffaro Spa Ind Chim | PROCEDURE FOR THE PREPARATION OF BASIC ALUMINUM COMPOUNDS. |
| US5938970A (en) * | 1997-06-11 | 1999-08-17 | General Chemical Corporation | Polynucleate metal hydroxide compounds and method for their preparation |
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| EP1108679A2 (en) | 2001-06-20 |
| DK1108679T3 (en) | 2004-02-02 |
| ATE251598T1 (en) | 2003-10-15 |
| EP1108679B1 (en) | 2003-10-08 |
| EP1108679A3 (en) | 2001-07-25 |
| NO20006218L (en) | 2001-06-18 |
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