NO301222B1 - Process for preparing homogeneous, fine, powdery solid dispersions, and using the dispersions - Google Patents
Process for preparing homogeneous, fine, powdery solid dispersions, and using the dispersions Download PDFInfo
- Publication number
- NO301222B1 NO301222B1 NO924190A NO924190A NO301222B1 NO 301222 B1 NO301222 B1 NO 301222B1 NO 924190 A NO924190 A NO 924190A NO 924190 A NO924190 A NO 924190A NO 301222 B1 NO301222 B1 NO 301222B1
- Authority
- NO
- Norway
- Prior art keywords
- substances
- finely dispersed
- clay
- solid
- active substances
- Prior art date
Links
- 239000007962 solid dispersion Substances 0.000 title claims description 47
- 238000004519 manufacturing process Methods 0.000 title claims description 20
- 239000006185 dispersion Substances 0.000 title description 5
- 239000000126 substance Substances 0.000 claims description 62
- 239000007787 solid Substances 0.000 claims description 57
- 239000013543 active substance Substances 0.000 claims description 48
- 239000000725 suspension Substances 0.000 claims description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 41
- 239000004927 clay Substances 0.000 claims description 40
- 238000000034 method Methods 0.000 claims description 34
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 33
- 239000000292 calcium oxide Substances 0.000 claims description 33
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 33
- 238000006243 chemical reaction Methods 0.000 claims description 32
- 229910052782 aluminium Inorganic materials 0.000 claims description 27
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 27
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 23
- 230000002209 hydrophobic effect Effects 0.000 claims description 17
- 239000010426 asphalt Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 14
- 150000001875 compounds Chemical class 0.000 claims description 11
- 238000001556 precipitation Methods 0.000 claims description 11
- -1 silicic acid ester Chemical class 0.000 claims description 11
- 235000012239 silicon dioxide Nutrition 0.000 claims description 9
- 238000001179 sorption measurement Methods 0.000 claims description 9
- 238000010521 absorption reaction Methods 0.000 claims description 8
- 238000004061 bleaching Methods 0.000 claims description 8
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical class O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 8
- 239000011573 trace mineral Substances 0.000 claims description 8
- 235000013619 trace mineral Nutrition 0.000 claims description 8
- 239000003153 chemical reaction reagent Substances 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 4
- 238000001784 detoxification Methods 0.000 claims description 3
- 235000013312 flour Nutrition 0.000 claims description 3
- 238000011065 in-situ storage Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- 230000000274 adsorptive effect Effects 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 claims description 2
- 238000005695 dehalogenation reaction Methods 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 229910052736 halogen Inorganic materials 0.000 claims description 2
- 150000002367 halogens Chemical class 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 claims description 2
- 239000012188 paraffin wax Substances 0.000 claims description 2
- 235000021317 phosphate Nutrition 0.000 claims description 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims description 2
- 229940099259 vaseline Drugs 0.000 claims description 2
- 238000007130 inorganic reaction Methods 0.000 claims 2
- 238000002955 isolation Methods 0.000 claims 1
- 238000006053 organic reaction Methods 0.000 claims 1
- 239000011814 protection agent Substances 0.000 claims 1
- 150000003568 thioethers Chemical class 0.000 claims 1
- 229910001385 heavy metal Inorganic materials 0.000 description 13
- 239000002689 soil Substances 0.000 description 9
- 239000003513 alkali Substances 0.000 description 7
- 235000014113 dietary fatty acids Nutrition 0.000 description 7
- 239000000194 fatty acid Substances 0.000 description 7
- 229930195729 fatty acid Natural products 0.000 description 7
- 150000004665 fatty acids Chemical class 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 7
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 description 6
- 239000005569 Iron sulphate Substances 0.000 description 6
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical class [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 6
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 6
- 239000000920 calcium hydroxide Substances 0.000 description 6
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 239000000428 dust Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 150000004763 sulfides Chemical class 0.000 description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 5
- 150000001412 amines Chemical class 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 238000000265 homogenisation Methods 0.000 description 5
- 238000006703 hydration reaction Methods 0.000 description 5
- 235000011837 pasties Nutrition 0.000 description 5
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 4
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric Acid Chemical compound [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 238000004898 kneading Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000004056 waste incineration Methods 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000002956 ash Substances 0.000 description 3
- 239000002361 compost Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 235000014413 iron hydroxide Nutrition 0.000 description 3
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical class [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 3
- 230000002427 irreversible effect Effects 0.000 description 3
- 230000007774 longterm Effects 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 3
- 239000011975 tartaric acid Substances 0.000 description 3
- 235000002906 tartaric acid Nutrition 0.000 description 3
- 231100000331 toxic Toxicity 0.000 description 3
- 230000002588 toxic effect Effects 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000440 bentonite Substances 0.000 description 2
- 229910000278 bentonite Inorganic materials 0.000 description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 238000005056 compaction Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- TXCDCPKCNAJMEE-UHFFFAOYSA-N dibenzofuran Chemical compound C1=CC=C2C3=CC=CC=C3OC2=C1 TXCDCPKCNAJMEE-UHFFFAOYSA-N 0.000 description 2
- 150000004826 dibenzofurans Chemical class 0.000 description 2
- 150000002013 dioxins Chemical class 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000003673 groundwater Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 235000013980 iron oxide Nutrition 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 239000012074 organic phase Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000003415 peat Substances 0.000 description 2
- 150000003071 polychlorinated biphenyls Chemical class 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 239000010802 sludge Substances 0.000 description 2
- 239000010457 zeolite Substances 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- OGBQILNBLMPPDP-UHFFFAOYSA-N 2,3,4,7,8-Pentachlorodibenzofuran Chemical compound O1C2=C(Cl)C(Cl)=C(Cl)C=C2C2=C1C=C(Cl)C(Cl)=C2 OGBQILNBLMPPDP-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical class [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 description 1
- JPHMPWQBESMBJL-UHFFFAOYSA-N [N].[Ca] Chemical compound [N].[Ca] JPHMPWQBESMBJL-UHFFFAOYSA-N 0.000 description 1
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 description 1
- 239000011609 ammonium molybdate Substances 0.000 description 1
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 1
- 235000018660 ammonium molybdate Nutrition 0.000 description 1
- 229940010552 ammonium molybdate Drugs 0.000 description 1
- 230000003698 anagen phase Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000001934 delay Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 150000002240 furans Chemical class 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910000358 iron sulfate Inorganic materials 0.000 description 1
- 210000003127 knee Anatomy 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 235000007079 manganese sulphate Nutrition 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 230000005226 mechanical processes and functions Effects 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 239000001120 potassium sulphate Substances 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- JVUYWILPYBCNNG-UHFFFAOYSA-N potassium;oxido(oxo)borane Chemical compound [K+].[O-]B=O JVUYWILPYBCNNG-UHFFFAOYSA-N 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000001226 reprecipitation Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000010801 sewage sludge Substances 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- DAOVYDBYKGXFOB-UHFFFAOYSA-N tris(2-methylpropoxy)alumane Chemical compound [Al+3].CC(C)C[O-].CC(C)C[O-].CC(C)C[O-] DAOVYDBYKGXFOB-UHFFFAOYSA-N 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical class [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 235000009529 zinc sulphate Nutrition 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B1/00—Dumping solid waste
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/50—Mixing liquids with solids
- B01F23/51—Methods thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0248—Compounds of B, Al, Ga, In, Tl
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0277—Carbonates of compounds other than those provided for in B01J20/043
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0285—Sulfides of compounds other than those provided for in B01J20/045
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0292—Phosphates of compounds other than those provided for in B01J20/048
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Description
Foreliggende oppfinnelse angår en fremgangsmåte for fremstilling av homogene, pulverformige faststoffdispersjoner, som eventuelt kan inneholde virksomme substanser, samt anvendelse av dispersjonene. The present invention relates to a method for the production of homogeneous, powdery solid dispersions, which may possibly contain active substances, as well as the use of the dispersions.
Faststoffdispersjoner spiller en betydelig rolle i land-brukssammenheng og i teknikken. Eksempler er leirmeltyper som spiller en viktig rolle som grunnforbedringsmidler og også som adsorpsjonsmidler i industrielle prosesser. Når det skal fremstilles findisperse faststoffdispersjoner av findisperse, vannholdige forprodukter, for eksempel av naturlig leire, må det anvendes tørkeprosesser hvor varmekostnadene er høye, med en etterfølgende mekanisk homogenisering. Dersom det skal fremstilles findisperse faststoffdispersjoner av grovkornige faste stoffer eller faststoffkomponenter, er det nødvendvig med kostbare mekaniske knuse-, henholdsvis male-prosesser, for å oppnå faststoffdispersjoner som i høy grad er findisperse og homogene. Disse mekaniske prosesser har iallfall grenser ved at den på denne måte stoffspesifikk oppnåelige kornstørrelse utelukkende blir bestemt av de teknisk maksimalt oppnåelige skjærkrefter. Solid dispersions play a significant role in agriculture and in technology. Examples are types of clay flour that play an important role as soil improvers and also as adsorbents in industrial processes. When finely dispersed solid dispersions are to be produced from finely dispersed, water-containing precursors, for example from natural clay, drying processes must be used where the heat costs are high, with a subsequent mechanical homogenization. If finely dispersed solid dispersions of coarse-grained solids or solid components are to be produced, expensive mechanical crushing or grinding processes are necessary to obtain solid dispersions that are highly finely dispersed and homogeneous. In any case, these mechanical processes have limits in that the material-specific grain size that can be achieved in this way is exclusively determined by the technically maximally achievable shear forces.
Det er derfor oppfinnelsens oppgave å stille til disposisjon en fremgangsmåte ifølge hvilken svært homogene og findisperse faststoffdispersjoner lar seg fremstille uten anvendelse av spesielt kostnadskrevende teknikk. It is therefore the task of the invention to make available a method according to which very homogeneous and finely dispersed solid dispersions can be produced without the use of particularly costly techniques.
For å løse denne oppgave homogeniserer man en vannholdig, findispers faststoffsuspensjon mekanisk med et edukt av en kjemisk reaksjon som forbruker vann, for eksempel med et jordalkalioksyd eller et aluminiumalkoholat eller en kiselsyreester eller en blanding av disse forbindelser, og lar deretter homogenisatet reagere ut under forbruk av den støkiometrisk nødvendige vannmengde. Som vannforbrukene reaksjon velger man reaksjoner hvor det av eduktet dannes et findisperst faststoff; i henhold til dette oppstår jord-alkalihydroksyder, henholdsvis aluminiumhydroksyder, henholdsvis kiselsyre av de nevnte edukter. To solve this task, an aqueous, finely dispersed solid suspension is mechanically homogenized with an educt of a chemical reaction that consumes water, for example with an alkaline earth oxide or an aluminum alcoholate or a silicic acid ester or a mixture of these compounds, and then allows the homogenized to react during consumption of the stoichiometrically required amount of water. As the water consumption reaction, one chooses reactions where a finely dispersed solid is formed from the educt; according to this, alkaline earth hydroxides, respectively aluminum hydroxides, respectively silicic acid arise from the aforementioned educts.
Vannholdige, findisperse faststoffsuspensjoner som er brukbare for oppfinnelsens formål er suspensjoner av findisperse faste stoffer i vann. Med findisperse stoffer menes i oppfinnelsen stoffer med partikkelstørrelser i området fra > 0 til < 250 jxrn, fortrinnsvis i området fra 1 til 50 / xm, og som på grunn av sine strukturelle kjennetegn oppviser en god adsorpsjonsevne. Eksempler er sjiktsilikater, findispers kiselsyre, aluminiumoksyder og aluminiumhydroksyder, utfelt kritt og jernoksyder. Pastaformige blandinger av disse med vann betegnes her som findisperse faststoffsuspensjoner. Aqueous, finely dispersed solid suspensions that are usable for the purposes of the invention are suspensions of finely dispersed solids in water. Finely dispersed substances in the invention mean substances with particle sizes in the range from > 0 to < 250 µm, preferably in the range from 1 to 50 µm, and which, due to their structural characteristics, exhibit a good adsorption capacity. Examples are layer silicates, finely dispersed silicic acid, aluminum oxides and aluminum hydroxides, precipitated chalk and iron oxides. Paste-like mixtures of these with water are referred to here as finely dispersed solid suspensions.
Vannandelen i den findisperse faststoffsuspensjon kan variere innenfor vide grenser dersom det på den ene side er nok vann til stede for den etterfølgende kjemiske omsetning med et jordalkalioksyd eller aluminiumalkoholat og dersom det på den andre side ikke er mer vann til stede, noe som kan tillates ved fremstilling av en pulverformig faststoffdispersjon. Fortrinnsvis stilles vanninnholdet i den findisperse faststoffsuspensjon inn på en slik måte at det foreligger en pastøs masse som kan knas. The proportion of water in the finely dispersed solid suspension can vary within wide limits if, on the one hand, there is enough water present for the subsequent chemical reaction with an alkaline earth oxide or aluminum alcoholate and if, on the other hand, no more water is present, which can be allowed by production of a powdery solid dispersion. Preferably, the water content in the finely dispersed solid suspension is set in such a way that there is a pasty mass that can be crunched.
De vannholdige, findisperse faststoffsuspensjoner kan være av naturlig eller av industriell opprinnelse. En pastøs og knabar, vannholdig, findispers faststoffsuspensjon av naturlig opprinnelse er leire slik den utvinnes i gruver for fremstilling av leirgods, og s,om i uforandret tilstand kan anvendes ifølge oppfinnelsen. Blekejord og leirmel er av industriell opprinnelse; dersom man lager en deig av disse med vann, oppnår man vannholdige', findisperse faststoffsuspensjoner som likeledes er brukbare i henhold til oppfinnelsen . The aqueous, finely dispersed solid suspensions can be of natural or industrial origin. A pasty and crunchy, water-containing, finely dispersed solid suspension of natural origin is clay as it is extracted in mines for the production of clay goods, and as such can be used in an unchanged state according to the invention. Bleaching earth and clay flour are of industrial origin; if you make a dough of these with water, you obtain water-containing, finely dispersed solid suspensions which are likewise usable according to the invention.
I tillegg til leire kan også leirlignende og leirholdige materialer anvendes for fremstilling av vannholdige, findisperse faststoffsuspensjoner. Når det her er tale om leirlignende og leirholdige materialer, så menes med dette utelukkende materialenes adsorpsjonsevne på grunn av fysikalsk-strukturelle kjennetegn og ikke den kjemiske sammensetning. Eksempler er leirholdige eller leirlignende flyvestøvtyper, filterstøvtyper, asketyper og produksjonsrester, for eksempel produksjonsrester fra næringsmiddelindustri i form av brukt blekejord, eller for eksempel rødslam, en pastøs masse som overveiende oppstår fra jernoksyder og jernhydroksyder i forbindelse med aluminiumfremstillingen. In addition to clay, clay-like and clay-containing materials can also be used for the production of aqueous, finely dispersed solid suspensions. When we are talking about clay-like and clay-containing materials, this means exclusively the adsorption capacity of the materials due to physical-structural characteristics and not the chemical composition. Examples are clayey or clay-like flying dust types, filter dust types, ash types and production residues, for example production residues from the food industry in the form of used bleaching earth, or for example red mud, a pasty mass that predominantly arises from iron oxides and iron hydroxides in connection with aluminum production.
Det hører til oppfinnelsens vesen at det vann som den findisperse faststoffsuspensjon inneholder, forbrukes på ensartet måte i den kjemiske reaksjon med jordalkalioksyd eller aluminiumalkoholat, fordi det bare under denne forutsetning kan oppstå en homogen, pulverformig faststoffdispersjon. Av denne grunn får den reaksjon som forbruker vann først begynne når eduktet av den vannforbrukende reaksjon er jevnt fordelt i faststoffsuspensjonen. Dette kan oppnås dersom man enten homogeniserer den vannholdige, findisperse faststoffsuspensjon med eduktet av den vannforbrukende reaksjon så hurtig at sistnevnte er jevnt fordelt i suspensjonen, før den vannforbrukende kjemiske reaksjon i nevneverdig grad begynner, eller ved at man til den vannholdige, findisperse faststoffsuspensjon setter til kjente reaksjonsforsinkende forbindelser, for eksempel ammoniakkløsning, alkoholer, alkalisulfater og lignende, eller at man forbehandler eduktet av den vannforbrukende reaksjon på tilsvarende måte, for eksempel med alkohol eller med langkjedede aminer, fettsyrer og lignende. I stedet for de rene edukter jordalkalioksyd eller aluminiumalkoholat eller kiselsyreester kan man også anvende blandinger av jordalkalioksyder eller aluminiumalkoholater eller kiselsyreestere eller blandinger av disse forbindelsesklasser. It belongs to the essence of the invention that the water which the finely dispersed solid suspension contains is consumed uniformly in the chemical reaction with alkaline earth oxide or aluminum alcoholate, because only under this condition can a homogeneous, powdery solid dispersion occur. For this reason, the water-consuming reaction may only begin when the educt of the water-consuming reaction is evenly distributed in the solid suspension. This can be achieved by either homogenizing the water-containing, finely dispersed solid suspension with the educt of the water-consuming reaction so quickly that the latter is evenly distributed in the suspension, before the water-consuming chemical reaction begins to an appreciable extent, or by adding to the aqueous, finely dispersed solid suspension known reaction-delaying compounds, for example ammonia solution, alcohols, alkali sulphates and the like, or that one pre-treats the educt of the water-consuming reaction in a similar way, for example with alcohol or with long-chain amines, fatty acids and the like. Instead of the pure educts alkaline earth oxide or aluminum alcoholate or silicic acid ester, one can also use mixtures of alkaline earth oxides or aluminum alcoholates or silicic acid esters or mixtures of these compound classes.
Produktene av leire som oppnås ifølge oppfinnelsen lar seg anvende som grunnforbedringsmidler eller som jordbygge-stoff, for eksempel for tetting av deponier. Dette gjelder på samme måte for alle andre kjente faststoffsuspensjoner. Faststoffdispersjoner med aluminiumhydroksyd eller kiselsyre kan anvendes som virksomme adsorpsjonsmidler. Når det gjelder anvendelse av faststoffsuspensjonene/faststoffdisper-sjonene, vises det også til kravene 21-25. The clay products obtained according to the invention can be used as ground improvement agents or as earth building material, for example for sealing landfills. This applies in the same way to all other known solid suspensions. Solid dispersions with aluminum hydroxide or silicic acid can be used as effective adsorbents. Regarding the use of the solid suspensions/solid dispersions, reference is also made to claims 21-25.
Tallrike kjemiske og fysikalske egenskaper for virksomme stoffer på et fast bærerstoff endrer seg i fordelaktig retning i avhengighet av dispersjonsgraden. Vanligvis tiltar den kjemiske reaktivitet jo finere fordelt et fast eller flytende stoff foreligger som reaksjonspartner på et bærerstoff. Fysikalsk sett endrer seg for eksempel hastigheten for innstilling av likevekter, når det for eksempel gjelder adsorpsjons- eller oppløsningsprosesser. Med finfordelte virksomme stoffer på et fast bærerstoff muliggjøres kjemiske og fysikalske prosesser som ellers ikke finner sted eller bare forløper langsomt. Numerous chemical and physical properties of active substances on a solid carrier change in a beneficial direction depending on the degree of dispersion. Generally, the chemical reactivity increases the more finely divided a solid or liquid substance is present as a reaction partner on a carrier substance. In physical terms, for example, the rate of setting equilibria changes when, for example, adsorption or dissolution processes are concerned. With finely divided active substances on a solid carrier substance, chemical and physical processes are made possible which otherwise do not take place or only proceed slowly.
Som kjent kan faste og flytende virksomme stoffer på-bringes mekanisk på et fast bærerstoff ved sammenmaling. Man kan også impregnere et fast bærerstoff med en løsning av det virksomme stoff og deretter tørke suspensjonen. Egnede virksomme stoffer kan dampes på et fast bærerstoff. Til sist består den mulighet å overføre virksomme stoffer i løpet av en dispergerende kjemisk reaksjon i et fast bærerstoff på homogen og findispers måte. As is known, solid and liquid active substances can be mechanically applied to a solid carrier substance by grinding together. You can also impregnate a solid carrier with a solution of the active substance and then dry the suspension. Suitable active substances can be vaporized on a solid carrier substance. Finally, there is the possibility of transferring active substances during a dispersing chemical reaction in a solid carrier substance in a homogeneous and finely dispersed manner.
De nevnte fremgangsmåter har når det gjelder anvendbar-heten bestemte begrensninger eller oppviser andre ulemper. Det finnes således grenser for maling av virksomme stoffer, ettersom de mekanisk oppnåelige skjærkrefter ikke strekker til for å oppnå en hvilken som helst vidtgående fineste fordeling av de virksomme stoffer i det malte produkt. Fremstillingen av homogent belastede, pulverformige faststoffdispersjoner under anvendelse av en løsning av det virksomme stoff eller ved pådamping er begrenset til løselige, henholdsvis fordampbare virksomme stoffer på grunn av den nød-vendige tekniske innsats, som vanligvis også er kostbar. Den homogene fineste fordeling av virksomme stoffer i løpet av dispergerende kjemiske reaksjoner er begrenset til virk-stoffer som kan for-fordeles i eduktet av den dispergerende kjemiske reaksjon. I tillegg kommer at disse edukter, nemlig jordalkalioksyder, aluminiumalkoholater og kiselsyreestere er relativt kostbare. The methods mentioned have certain limitations in terms of applicability or exhibit other disadvantages. There are thus limits to the painting of active substances, as the mechanically achievable shear forces are not sufficient to achieve any far-reaching finest distribution of the active substances in the painted product. The production of homogeneously loaded, powdery solid dispersions using a solution of the active substance or by evaporation is limited to soluble, respectively vaporizable active substances due to the necessary technical effort, which is usually also expensive. The homogeneous finest distribution of active substances during dispersing chemical reactions is limited to active substances that can be distributed in the educt of the dispersing chemical reaction. In addition, these educts, namely alkaline earth oxides, aluminum alcoholates and silicic acid esters are relatively expensive.
Oppfinnelsen har derfor stilt seg den ytterligere oppgave å fremstille pulverformige faststoffdispersjoner som er homogent belastet med virksomme stoffer, på teknisk enkel og derfor også økonomisk måte, og under vidtgående unngåelse av begrensninger og ulemper. The invention has therefore set itself the further task of producing powdery solid dispersions which are homogeneously loaded with active substances, in a technically simple and therefore also economical way, and while largely avoiding limitations and disadvantages.
For å løse denne oppgave er det funnet en fremgangsmåte for fremstilling av homogene, findisperse faststoffdispersjoner,karakterisert vedat man mekanisk homogeniserer en vannholdig, findispers faststoffsuspensjon med et jordalkalioksyd, aluminiumalkoholat, kiselsyreester eller en blanding av disse forbindelser, og deretter lar homogenisatet reagere ut med den støkiometrisk nødvendige vannmengde. In order to solve this task, a method has been found for the production of homogeneous, finely dispersed solid dispersions, characterized by mechanically homogenizing an aqueous, finely dispersed solid suspension with an alkaline earth oxide, aluminum alcoholate, silicic acid ester or a mixture of these compounds, and then allowing the homogenized to react with the stoichiometrically required amount of water.
Ifølge oppfinnelsestanken nyttiggjøres den latent tilstedeværende adsorpsjonsevne hos de i en vannholdig fast-stof f suspensjon findisperst foreliggende faststoffer, som i disse omgivelser er fullstendig belagt med vann og således praktisk talt ikke er i stand til adsorpsjon, dersom man på kjemisk måte trekker ut vannet av den vannholdige faststoffsuspensjon i nærvær av adsorberbare, virksomme stoffer som foreligger i homogen fordelt form og som kan foreligge som løsning i en findispers suspensjon, ved hjelp av en reaksjon som forbruker vann, eksempelvis ved hjelp av en jordalkali-oksydhydratasjonsreaksjon eller ved hydrolyse av et aluminiumalkoholat, slik at de virksomme stoffer blir bundet på adsorptiv måte på overflaten av det nå i høy grad vannfrie faste stoff. Det hører med til oppfinnelsens vesen at det findisperse, faste reaksjonsprodukt, eksempelvis findisperst jordalkali-, henholdsvis aluminiumhydroksyd av jordalkalioksyd, henholdsvis aluminiumalkoholat som samtidig oppstår av eduktet av en reaksjon som forbruker vann, likeledes blir adsorptivt virksomt. According to the idea of the invention, the latently present adsorption capacity of the finely dispersed solids present in an aqueous solid f suspension, which in these environments are completely covered with water and are thus practically incapable of adsorption, is utilized if the water is chemically extracted from the aqueous solid suspension in the presence of adsorbable, active substances which are present in homogeneously distributed form and which can be present as a solution in a finely dispersed suspension, by means of a reaction that consumes water, for example by means of an alkaline earth oxide hydration reaction or by hydrolysis of an aluminum alcoholate , so that the active substances are bound in an adsorptive manner on the surface of the now largely anhydrous solid substance. It is part of the essence of the invention that the finely dispersed, solid reaction product, for example finely dispersed alkaline earth, respectively aluminum hydroxide of alkaline earth oxide, respectively aluminum alcoholate which simultaneously arises from the educt of a reaction that consumes water, likewise becomes adsorptively effective.
Fordelen med oppfinnelsen beror på at i motsetning til det som skjer ved mekanisk dispergering, er også små mengder virksomme stoffer homogent fordelbare på et fast bærerstoff, og at i motsetning til det som finner sted ved en homogen fineste fordeling av virksomme stoffer under forløpet av dispergerende kjemiske reaksjoner den i det tilfelle ufra-vikelige forutsetning, nemlig at forfordelingsevnen i eduktet av den dispergerende kjemiske reaksjon for de virksomme stoffer som skal fordeles, for eksempel i et jordalkalioksyd, aluminiumalkoholat eller kiselsyreester, absolutt ikke er nødvendig. Stikk motsatt homogeniseres ifølge oppfinnelsen for fremstilling av en med virksomme stoffer homogent belastet, pulverformig faststoffdispersjon, det virksomme stoff på mekanisk måte med en vannholdig, findispers faststoffsuspensjon, og homogenisatet homogeniseres først deretter med et jordalkalioksyd eller aluminiumalkoholat. På denne måte kan den andel av jordalkalioksyd eller aluminiumalkoholat som er nødvendig for fremstilling av en pulverformig faststoffdispersjon som er homogent belastet med virksomme stoffer, reduseres i betraktelig grad og i gunstige tilfeller til ca. en tiendedel av den for en dispergerende kjemisk reaksjon nødvendige mengde. The advantage of the invention lies in the fact that, in contrast to what happens with mechanical dispersion, even small amounts of active substances are homogeneously distributed on a solid carrier substance, and that in contrast to what takes place in the case of a homogeneous fine distribution of active substances during the course of dispersing chemical reactions the invariable condition in that case, namely that the ability to predistribute in the educt of the dispersing chemical reaction for the active substances to be distributed, for example in an alkaline earth oxide, aluminum alcoholate or silicic acid ester, is absolutely not necessary. On the contrary, according to the invention, for the production of a powdered solid dispersion homogeneously loaded with active substances, the active substance is mechanically homogenized with an aqueous, finely dispersed solid suspension, and the homogenized is only then homogenized with an alkaline earth oxide or aluminum alcoholate. In this way, the proportion of alkaline earth oxide or aluminum alcoholate that is necessary for the production of a powdery solid dispersion that is homogeneously loaded with active substances can be reduced to a considerable extent and in favorable cases to approx. one tenth of the quantity required for a dispersing chemical reaction.
Som virksomme stoffer betegnes her stoffer som, i motsetning til de stoffer i faststoffsuspensjonen som utelukkende anses som bærerstoff, er spesielt virksomme på kjemisk og fysikalsk måte i den finfordelte tilstand. Også i denne sammenheng kommer det ikke an på de fysikalske og kjemiske egenskaper for de deltagende stoffer i seg selv, bare med henblikk på den rolle som disse tilordnes for den anvendelse som til enhver tid finner sted. Dette skal for-klares på grunnlag av to eksempler. Active substances are defined here as substances which, in contrast to the substances in the solid suspension which are considered exclusively as carrier substances, are particularly active chemically and physically in the finely divided state. Also in this context, it does not depend on the physical and chemical properties of the participating substances themselves, only with regard to the role that these are assigned for the application that takes place at any given time. This will be explained on the basis of two examples.
Naturlig leire homogeniseres med en konsentrert vandig løsning av natriumsulfid ved knaing; den plastiske masse som oppstår gir i den etterfølgende vannforbrukende kjemiske omsetning med ca. 15% hydrofobt kalsiumklorid, beregnet på den anvendte leirmengde, en med sulfidioner homogent belastet pulverformig faststoffdispersjon. Det finfordelte virksomme stoff i form av sulfidioner utgjør som bekjent en høyreaktiv utfellingsreagens, ved hjelp av hvilken tallrike toksiske tungmetaller ved utfelling lar seg overføre i vannuløselige tungmetallsulfider, slik at de på denne måte lar seg fiksere og immobilisere. For dette formål blander man tungmetall-kontaminert jordsmonn, flyveaske, slagg, med den nevnte fast-stof f dispers j on og komprimerer deretter til et faststoff-legeme. Kontaminerte materialer i form av grove stykker, for eksempel skorstenskledninger, fundamentdeler, utrustning og lignende, innleires i den nevnte faststoffdispersjon i den form de forekommer, eller i blanding under komprimering med andre materialer som er fordelaktige når det gjelder grunnens eller jordsmonnets mekaniske egenskaper. Det grunnmekaniske aspekt spiller en spesielt viktig rolle ved behandlingen av tungmetall-forurensede klaringsslam med sine grunn-mekanisk ustabile gelstrukturer, for at de etter homogeniseringen med den nevnte faststoffdispersjon på sikker måte skal kunne lagres i form av grunn-mekanisk stabile grunnlegemer med bæreevne. I dette tilfelle er innblanding av egnede, tungmetall-kontaminerte avfallsstoffer, så som slagg og aske, samfunnsøkonomisk spesielt fordelaktig. Natural clay is homogenized with a concentrated aqueous solution of sodium sulphide by kneading; the plastic mass that occurs gives in the subsequent water-consuming chemical reaction with approx. 15% hydrophobic calcium chloride, calculated on the amount of clay used, a powdery solid dispersion homogeneously loaded with sulphide ions. The finely divided active substance in the form of sulphide ions constitutes, as is well known, a highly active precipitation reagent, with the help of which numerous toxic heavy metals can be transferred during precipitation into water-insoluble heavy metal sulphides, so that they can be fixed and immobilized in this way. For this purpose, heavy metal-contaminated soil, fly ash, slag are mixed with the aforementioned solid dispersion and then compressed into a solid body. Contaminated materials in the form of rough pieces, for example chimney linings, foundation parts, equipment and the like, are embedded in the aforementioned solid dispersion in the form in which they occur, or mixed during compaction with other materials that are advantageous in terms of the mechanical properties of the ground or soil. The basic mechanical aspect plays a particularly important role in the treatment of heavy metal-contaminated clarification sludge with its basic-mechanically unstable gel structures, so that, after homogenization with the aforementioned solid dispersion, they can be safely stored in the form of basic-mechanically stable basic bodies with load-bearing capacity. In this case, mixing in suitable, heavy-metal-contaminated waste materials, such as slag and ash, is particularly beneficial from a socio-economic perspective.
Ifølge en spesielt virksom fremgangsmåtevariant knas først en delmengde av leiren med en vandig alkalisk sulfid-løsning og en andre delmengde med en finkornet vandig suspensjon av jernsulfat. Når man deretter homogeniserer begge delmengder så oppstår in situ svært fint fordelt jernsulfid som er innleiret i leirstrukturen. Den ennå pastøse masse omsettes nå kjemisk med ca. 2 0%, beregnet på den samlede leirmengde, normalt, dvs. ikke hydrofobert kalsiumoksyd. De støkiometriske mengdeforhold velges på en slik måte at det foreligger et lite overskudd av jernioner, for eksempel 10%. Det virksomme stoff består nå av jernsulfid, som går for å være vannuløselig. På grunn av det svært mye lavere løselig-hetsprodukt for sulfidene av toksiske tungmetaller finner det imidlertid etter innblanding i tungmetallkontaminerte materialer sted en omfelling. På denne måte muliggjøres en spesielt virksom tungmetall-immobilisering uten at det er fare for grunnvannet dersom mobile, dvs. vannløselige, alkalisulfider anvendes direkte. According to a particularly effective method variant, a portion of the clay is first crushed with an aqueous alkaline sulphide solution and a second portion with a fine-grained aqueous suspension of iron sulphate. When both sub-quantities are then homogenised, very finely distributed iron sulphide occurs in situ, which is embedded in the clay structure. The still pasty mass is now chemically reacted with approx. 20%, calculated on the total amount of clay, normal, i.e. non-hydrophobic calcium oxide. The stoichiometric quantity ratios are chosen in such a way that there is a small excess of iron ions, for example 10%. The active substance now consists of iron sulphide, which is supposed to be water insoluble. However, due to the very much lower solubility product for the sulphides of toxic heavy metals, a reprecipitation takes place after mixing in heavy metal-contaminated materials. In this way, a particularly effective heavy metal immobilization is made possible without there being any danger to the groundwater if mobile, i.e. water-soluble, alkali sulphides are used directly.
I det forannevnte eksempel og i den tilhørende fremgangsmåtevariant anvendes det sammen med de nevnte sulfider stoffer som på grunn av sin kjemiske reaktivitet, i hovedsak som fellingsreagens, uten videre kan kalles virksomme stoffer. Virksomme stoffer i oppfinnelsens betydning kan imidlertid også være stoffer som kjemisk gjelder som inerte. In the above-mentioned example and in the associated method variant, substances which, due to their chemical reactivity, mainly as precipitation reagents, can easily be called active substances are used together with the aforementioned sulphides. However, active substances in the meaning of the invention can also be substances that are chemically regarded as inert.
Dersom man for eksempel smelter opp hardbitumen, knar den med leire og til denne masse, straks den er homogen, tilsetter kalsiumoksyd, fortrinnsvis hydrofobt kalsiumoksyd og igjen knar den, så inntrer etter en tid kalsiumoksydets vannforbrukende hydratasjonsreaksjon, og den opprinnelig pastøse masse faller fra hverandre til en med hardbitumen homogent belastet, pulverformig faststoffdispersjon. Det kalsiumhydroksyd som denne faststoffdispersjon inneholder er som kjent på ingen måte inert i kjemisk henseende, men har sterkt basiske egenskaper og lar seg derfor lett omsette, for eksempel med karbondioksyd, mens det hardbitumen som likeledes befinner seg i denne faststoffdispersjon kjemisk sett er fullstendig inert. If, for example, you melt the hard bitumen, knead it with clay and to this mass, as soon as it is homogeneous, add calcium oxide, preferably hydrophobic calcium oxide and knead it again, then after a while the calcium oxide's water-consuming hydration reaction takes place, and the originally pasty mass falls apart to a powdery solid dispersion loaded homogeneously with the hard bitumen. As is known, the calcium hydroxide that this solid dispersion contains is in no way chemically inert, but has strongly basic properties and can therefore be easily reacted, for example with carbon dioxide, while the hard bitumen which is likewise found in this solid dispersion is chemically completely inert.
Likevel er den i faststoffdispersjonen tilstedeværende blanding av leirpartikler og kalsiumhydroksyd bærerstoffet og hardbitumen er det virksomme stoff, dersom oppgaven for eksempel består i å uskadeliggjøre i høy grad giftige organiske skadelige stoffer, som polyklorerte bifenyler (PCB) eller dioksiner og dibenzofuran (PCDD/PCDF), for eksempel i form av innholdsstoffer i filterstøv fra søppelforbrennings-anlegg eller som forurensning i jordsmonn, gjennom en irreversibel immobilisering. For dette formål blander man flyvestøv som er kontaminert på denne måte, eller jordsmonn, med en pulverformig faststoffdispersjon som er belastet med hardbitumen og som er blitt fremstilt under anvendelse av leire og kalsiumoksyd, og fremstiller av blandingen et jords-monnlegeme ved komprimering. Det findisperse hardbitumen i faststoff-matriksen har etter kort tid inkorporert de organiske skadelige stoffer, på grunn av disse stoffers gode løselighet i det faste løsemiddel hardbitumen. Utlutings-forsøk under langtidsbetingelser og under anvendelse av sporanalytiske metoder beviser at på denne måte ifølge oppfinnelsen behandlede organiske skadelige stoffer forblir varig og fullstendig immobilisert. I stedet for hardbitumen kan det også anvendes andre høytkokende organiske inert-stoffer, så som hardparaffin, vaselin eller mineralolje. Nevertheless, the mixture of clay particles and calcium hydroxide present in the solid dispersion is the carrier substance and the hard bitumen is the active substance, if the task, for example, consists of neutralizing highly toxic organic harmful substances, such as polychlorinated biphenyls (PCB) or dioxins and dibenzofuran (PCDD/PCDF) , for example in the form of constituents in filter dust from waste incineration plants or as contamination in soil, through an irreversible immobilisation. For this purpose, flying dust that is contaminated in this way, or soil, is mixed with a powdery solid dispersion loaded with hard bitumen and which has been produced using clay and calcium oxide, and a soil body is produced from the mixture by compaction. The finely dispersed hard bitumen in the solid matrix has after a short time incorporated the organic harmful substances, due to the good solubility of these substances in the solid solvent hard bitumen. Leaching tests under long-term conditions and using trace analytical methods prove that organic harmful substances treated in this way according to the invention remain permanently and completely immobilized. Instead of hard bitumen, other high-boiling organic inert substances can also be used, such as hard paraffin, vaseline or mineral oil.
En oppramsing av de enkelte virksomme stoffer og blandinger av virksomme stoffer er umulig, ettersom utvalgejfc|g^£§^av slike gir seg selv ifølge aspekter som forekommer i for- '" bindelse med de oppgaver som til enhver tid stilles. Det er eksempelvis kjent at det ved fremstilling av plantesubstrater er nødvendig med sporelementer i forskjellig konsentrasjon og biologisk tilgjengelighet. Til disse regnes kobber, jern, mangan, sink, molybden og bor, idet de vannløselige forbindelser av disse anvendes i mekanisk blanding og i form av heterogene konsentrater. Disse preparaters ulemper består i at de nevnte sporelementer ikke står til jevn disposisjon for planten, fordi en jevn fordeling i substratet er utelukket. Dersom man i motsetning til dette først knar de samme forbindelser av de nevnte sporelementer inn i en leirmatriks, slik at de på denne måte fordeles jevnt, så oppnår man etter homogenisering av denne blanding med kalsiumoksyd en ytterst findispers faststofftilberedning i hvilken de virksomme stoffer forekommer ekstremt ensartet. Ved meddispergering av vin- og sitronsyre er det mulig på forhånd å bestemme de nevnte sporelementers biologiske tilgjengelighet. Dersom man overfører sporelement-forbindelsene, med eller uten vinsyre, enkeltvis i en pulverformig faststoffdispersjon og først senere vil blande i det til enhver tid nødvendige mengdeforhold for anvendelse, så anbefales dessuten medfordeling av et hydrofoberingsmiddel, fordi det da i blandingen av de enkelte pulverformige faststoffdispersjoner ikke er mulig med ufordelaktige vekselvirkninger av sporelementenes forbindelser med hverandre. An enumeration of the individual active substances and mixtures of active substances is impossible, as the selection of such gives itself according to aspects that occur in connection with the tasks that are set at any given time. There is, for example it is known that in the production of plant substrates, trace elements in different concentrations and biological availability are needed. These include copper, iron, manganese, zinc, molybdenum and boron, as the water-soluble compounds of these are used in mechanical mixing and in the form of heterogeneous concentrates. The disadvantages of these preparations consist in the fact that the mentioned trace elements are not evenly available to the plant, because an even distribution in the substrate is excluded. If, in contrast to this, the same compounds of the mentioned trace elements are first kneaded into a clay matrix, so that they distributed evenly in this way, then after homogenization of this mixture with calcium oxide, an extremely finely dispersed solid preparation is obtained in which the active substances occur extremely uniformly. By co-dispersing tartaric and citric acid, it is possible to determine in advance the biological availability of the mentioned trace elements. If one transfers the trace element compounds, with or without tartaric acid, individually in a powdery solid dispersion and only later wants to mix in the quantity ratio required at all times for use, then co-distribution of a hydrophobic agent is also recommended, because then in the mixture of the individual powdery solid dispersions is not possible with unfavorable interactions of the trace elements' connections with each other.
På samme måte kan plantenæringsstoffer av de for-skjelligste typer bearbeides til svært homogene langtids-gjødseltyper, dersom de er holdbare i det alkaliske medium som oppstår. In the same way, plant nutrients of the most different types can be processed into very homogeneous long-term fertilizer types, if they are durable in the alkaline medium that occurs.
Tallet på anvendbare virksomme stoffer i miljø-beskyttelsesområdet er uoversiktelig stort, ettersom tallet på problematiske skadelige stoffer er så stort. Teoretisk finnes det for hvert skadelig stoff, i det minste imidlertid for hver klasse av skadelige stoffer, virksomme stoffer i henhold til oppfinnelsen som kan anvendes som reaksjonspartner, for eksempel som fellings-, kondensasjons- eller addisjonspartner, for immobilisering og avgifting, for bare å ha nevnt noen eksempler. I denne sammenheng får høytkokende organiske faser en spesiell betydning for adsorpsjon, henholdsvis absorpsjon, av såvel uorganiske som organiske skadelige stoffer, fordi denne form for immobilisering og fysikalske fiksering er spesielt enkel og omfattende. Et eksempel blant flere er den absorptive fjerning av skadelige stoffer fra avgasser fra søppelforbrenningsanlegg ved hjelp av langkjedede aminer som virksomme stoffer. I tillegg lar det seg også i den organiske fase innarbeide ytterligere virksomme stoffer som er i stand til kjemisk vekselvirkning med skadelige stoffer og som derfor forskyver likevekts-stillingen slik at en fullstendig absorpsjon begunstiges, for eksempel ved hjelp av langkjedede aminer i en bituminøs fase. Sammenhengen mellom virksomme stoffer som kan velges ut og den oppgave som skal løses er kjent for enhver fagmann og behøver derfor ingen ytterligere forklaring. Enhver fagmann kjenner således til at findisperse metaller, så som magnesium eller aluminium, lar seg anvende til dehalogenering av halogenholdige aromater. The number of applicable active substances in the area of environmental protection is unmanageably large, as the number of problematic harmful substances is so large. Theoretically, there are for each harmful substance, at least for each class of harmful substances, active substances according to the invention that can be used as reaction partners, for example as precipitation, condensation or addition partners, for immobilization and detoxification, just to have mentioned some examples. In this context, high-boiling organic phases take on a special importance for adsorption, respectively absorption, of both inorganic and organic harmful substances, because this form of immobilization and physical fixation is particularly simple and comprehensive. One example among many is the absorptive removal of harmful substances from exhaust gases from waste incineration plants using long-chain amines as active substances. In addition, it is also possible to incorporate further active substances in the organic phase which are capable of chemical interaction with harmful substances and which therefore shift the equilibrium position so that complete absorption is favoured, for example with the help of long-chain amines in a bituminous phase. The connection between active substances that can be selected and the task to be solved is known to any expert and therefore needs no further explanation. Anyone skilled in the art thus knows that finely dispersed metals, such as magnesium or aluminium, can be used for dehalogenation of halogen-containing aromatics.
I det i det foregående anførte andre eksempel, hvor an-vendelsen av hardbitumen som virksomt stoff ble forklart, anvendes fortrinnsvis hydrofobt kalsiumoksyd. Det hører til oppfinnelsens vesen at det i den findisperse faststoffsuspensjon forekommende vann forbrukes på ensartet vis i den kjemiske reaksjon med jordalkalioksyd eller aluminiumalkoholat, ettersom det bare under denne forutsetning kan oppstå en homogent belastet pulverformig faststoffdispersjon. Av denne grunn får den reaksjon som forbruker vann først begynne når jordalkalioksydet eller aluminiumalkoholatet er ensartet fordelt i homogenisatet av virksom forbindelse og faststoffsuspensjon. Dette lar seg oppnå dersom man enten homogeniserer homogenisatet av vannholdig, findispers fast-stof f suspens j on og virksomme stoffer så hurtig med jordalkalioksydet eller aluminiumalkoholatet at sistnevnte fordeles jevnt i homogenisatet, før den vannforbrukende kjemiske reaksjon begynner i nevneverdig omfang, eller ved at man til den vannholdige, findisperse faststoffsuspensjon tilsetter kjente reaksjonsforsinkere, for eksempel ammoniakkløsning, alkoholer, alkalisulfater og lignende, eller at man forbehandler jordalkalioksydet eller aluminiumalkoholatet på tilsvarende måte, for eksempel med alkohol eller langkjedede aminer, fettsyrer og lignende. In the second example mentioned above, where the use of hard bitumen as an active substance was explained, hydrophobic calcium oxide is preferably used. It belongs to the essence of the invention that the water present in the finely dispersed solid suspension is consumed in a uniform manner in the chemical reaction with alkaline earth oxide or aluminum alcoholate, as only under this condition can a homogeneously loaded powdery solid dispersion occur. For this reason, the reaction that consumes water can only begin when the alkaline earth oxide or aluminum alcoholate is uniformly distributed in the homogenize of active compound and solid suspension. This can be achieved if you either homogenize the homogenise of aqueous, finely dispersed solid suspension and active substances so quickly with the alkaline earth oxide or the aluminum alcoholate that the latter is distributed evenly in the homogenise, before the water-consuming chemical reaction begins to an appreciable extent, or by to the water-containing, finely dispersed solid suspension, known reaction retarders are added, for example ammonia solution, alcohols, alkali sulphates and the like, or that the alkaline earth oxide or aluminum alcoholate is pretreated in a similar way, for example with alcohol or long-chain amines, fatty acids and the like.
I stedet for de rene jordalkalioksyder eller aluminiumalkoholater kan man også anvende blandinger av jordalkalioksyder eller aluminiumalkoholater eller blandinger av begge forbindelsesklasser. Instead of the pure alkaline earth oxides or aluminum alcoholates, mixtures of alkaline earth oxides or aluminum alcoholates or mixtures of both compound classes can also be used.
For anvendelse av slike pulverformige faststoffsuspensjoner som er homogent belastet med virksomme substanser for landbruksformål eller for tekniske formål, spesielt også innenfor området miljøvern, er det fordelaktig dersom man gjennom en passende prosessføring eller ved etterfølgende blanding innstiller et overskudd av kalsiumoksyd, fortrinnsvis av hydrofobt kalsiumoksyd. På denne måte kan seige (tysk: bindige) kontaminerte materialer oppsluttes i en arbeidsgang, slik at de virksomme stoffer fordeler seg ensartet i mediet og slik at de skadelige stoffer opptas fullstendig og gjøres uskadelige. For the use of such powdery solid suspensions which are homogeneously loaded with active substances for agricultural purposes or for technical purposes, especially also within the area of environmental protection, it is advantageous if, through a suitable process or subsequent mixing, an excess of calcium oxide, preferably of hydrophobic calcium oxide, is introduced. In this way, tough (German: binding) contaminated materials can be contained in one work step, so that the active substances are distributed uniformly in the medium and so that the harmful substances are completely absorbed and rendered harmless.
Eksempel 1 Example 1
100 vektdeler av en naturlig plastisk leire homogeniseres i en knainnretning med 18 vektdeler av et kalsiumoksyd som var hydrofobert med 1% fettsyre. Man lar hydratasjonsreaksjonen, som begynner etter ca. 5 minutter, forløpe utenfor knainnretningen; på denne måte oppstår en ytterst homogen faststoffdispersjon av kalsiumhydroksyd i leire, som er så homogen at komponentene i seg selv ikke mer kan gjen-kjennes under mikroskopet. 100 parts by weight of a natural plastic clay are homogenized in a kneading device with 18 parts by weight of a calcium oxide which was hydrophobicized with 1% fatty acid. The hydration reaction, which begins after approx. 5 minutes, run outside the knee device; in this way, an extremely homogeneous solid dispersion of calcium hydroxide in clay is produced, which is so homogeneous that the components themselves can no longer be recognized under the microscope.
Variant Variant
Man knar den plastiske leire først med 2% kaliumsulfat som reaksjonsforsinker og deretter med ikke-hydrofobert kalsiumoksyd. Hydratasjonsreaksjonen begynner først etter ca. 2 0 minutter. The plastic clay is first kneaded with 2% potassium sulphate as a reaction retarder and then with non-hydrophobic calcium oxide. The hydration reaction only begins after approx. 20 minutes.
Variant Variant
I stedet for leire anvendes rødslam eller en til deig bearbeidet masse av 70 vektdeler tørr, brukt blekejord og 30 vektdeler vann. Instead of clay, red mud is used or a dough-processed mass of 70 parts by weight of dry, spent bleaching earth and 30 parts by weight of water.
Variant Variant
I stedet for kalsiumoksyd kan den støkiometriske ekvi-valent av aluminium-blandingsalkoholat, henholdsvis kiselsyreestere, finne anvendelse; i dette tilfelle fordamper den alkohol som settes fri i hydrolysen; den kan gjenvinnes ved kondensasj on. Instead of calcium oxide, the stoichiometric equivalent of aluminum mixture alcoholate, respectively silicic acid esters, can be used; in this case the alcohol liberated in the hydrolysis evaporates; it can be recovered by condensation.
Eksempel 2 Example 2
70 vektdeler leire, 7,6 vektdeler jernsulfat FeSO4-7H20, 3 vektdeler natriumsulfid Na2S (60%) og 4 vektdeler vann homogeniseres i en knainnretning. Homogenisatet homogeniseres med 15,4 vektdeler kalsiumoksyd. På denne måte oppstår 10 0 vektdeler av en med 2% jernsulfid homogent belastet pulverformig faststoffdispersjon, som kan anvendes for felling av tungmetaller i kontaminerte materialer. Andelen av jernsulfat er tilmålt slik at det foreligger et overskudd på 20% i forhold til den støkiometrisk nødvendige mengde; på denne måte forhindres at løselig alkalisulfid, for eksempel ved behandling av kontaminert grunn eller kontaminerte produksjonsrester, under forløpet av behandlingen ifølge oppfinnelsen kan komme inn i grunnvannet. Leiren i dette eksemplet kan helt eller delvis erstattes ved at tørr, brukt blekejord bearbeides til deig med vann, eksempelvis 77 vektdeler brukt blekejord fra næringsmiddelindustrien med 23 vektdeler vann, eller leiren kan erstattes med såkalt rødslam, eller ved at et findisperst filterstøv bearbeides til deig med så mye vann at det oppstår en leirlignende matriks. Tilsetning av reaksjonsforsinkere er i dette tilfelle ikke nødvendig, fordi jernsulfat i analogi til alkalisulfåtene allerede forsinker kalsiumoksydets kjemiske reaksjon i en slik grad at en fullstendig homogenisering er mulig før kalsiumoksydets vannforbrukende reaksjon begynner. 70 parts by weight of clay, 7.6 parts by weight of iron sulphate FeSO4-7H20, 3 parts by weight of sodium sulphide Na2S (60%) and 4 parts by weight of water are homogenised in a kneader. The homogenize is homogenized with 15.4 parts by weight of calcium oxide. In this way, 100 parts by weight of a powdery solid dispersion homogenously loaded with 2% iron sulphide is produced, which can be used for the precipitation of heavy metals in contaminated materials. The proportion of iron sulphate is measured so that there is an excess of 20% in relation to the stoichiometrically required amount; in this way, it is prevented that soluble alkali sulphide, for example during the treatment of contaminated soil or contaminated production residues, can enter the groundwater during the course of the treatment according to the invention. The clay in this example can be completely or partially replaced by dry, used bleaching earth being processed into dough with water, for example 77 parts by weight of used bleaching earth from the food industry with 23 parts by weight of water, or the clay can be replaced with so-called red mud, or by a finely dispersed filter dust being processed into dough with so much water that a clay-like matrix is formed. The addition of reaction retarders is not necessary in this case, because iron sulfate, in analogy to the alkali sulfates, already delays the calcium oxide's chemical reaction to such an extent that a complete homogenization is possible before the calcium oxide's water-consuming reaction begins.
Eksempel 3 Example 3
I en variant til eksempel 2 homogeniseres 3 5 vektdeler leire med en suspensjon av 7,6 vektdeler jernsulfat og 2 vektdeler vann i en tvangsblander. 35 vektdeler leire homogeniseres med en vandig løsning av 3 vektdeler natriumsulfid (60%) i 2 vektdeler vann i en tvangsblander. In a variant of example 2, 35 parts by weight of clay are homogenised with a suspension of 7.6 parts by weight of iron sulphate and 2 parts by weight of water in a forced mixer. 35 parts by weight of clay are homogenised with an aqueous solution of 3 parts by weight of sodium sulphide (60%) in 2 parts by weight of water in a forced mixer.
Begge disse andeler homogeniseres etter gjennomført homogenisering i en tvangsblander og homogeniseres deretter med 15,4 vektdeler hydrofobt kalsiumoksyd. Det oppstår en med 2% jernsulfid, FeS, ekstremt homogent belastet pulverformig faststoffdispersjon, som kan anvendes som dispersjonen ifølge eksempel 1. Both of these proportions are homogenized after completed homogenization in a forced mixer and then homogenized with 15.4 parts by weight of hydrophobic calcium oxide. An extremely homogenously charged powdery solid dispersion with 2% iron sulphide, FeS, is produced, which can be used as the dispersion according to example 1.
Eksempel 4 Example 4
I variant til eksempel 2, henholdsvis 3, homogeniseres de adskilt fremstilte homogenisater av leire og jernsulfat, henholdsvis av leire og natriumsulfid, med i hvert tilfelle 7,7 vektdeler kalsiumoksyd, henholdsvis hydrofobt kalsiumoksyd. Ved blanding av de to pulverformige faststoffdispersjoner som er homogent belastet med jernhydroksyd, henholdsvis natriumsulfid, oppnår man en tilberedning som i nærvær av et overskudd av hydrofobt kalsiumhydroksyd kan anvendes på spesielt virkningsfull og samtidig miljøvennlig måte for behandling av tungmetallholdige, seige materialer, fordi for det første fellingen av tungmetaller uopphørlig finner sted ved hjelp av alkalisulfidet og for det andre fordi ingen spor av dette sulfid kan nå ut i det omgivende miljø, fordi det oppfanges av det tilstedeværende jernhydroksyd uten at den utfellende virkning på tungmetaller som ennå ikke kan nås oppheves på grunn av dette. In a variation to example 2, respectively 3, the separately prepared homogenises of clay and iron sulphate, respectively of clay and sodium sulphide, are homogenised with in each case 7.7 parts by weight of calcium oxide, respectively hydrophobic calcium oxide. By mixing the two powdery solid dispersions which are homogeneously loaded with iron hydroxide and sodium sulphide respectively, a preparation is obtained which, in the presence of an excess of hydrophobic calcium hydroxide, can be used in a particularly effective and at the same time environmentally friendly way for the treatment of tough materials containing heavy metals, because for the first, the precipitation of heavy metals ceaselessly takes place with the help of the alkali sulphide and, secondly, because no trace of this sulphide can reach the surrounding environment, because it is captured by the iron hydroxide present without the precipitating effect on heavy metals which cannot yet be reached being canceled out on because of this.
Eksempel 5 Example 5
56 vektdeler leire plastifiseres med 15 vektdeler vann og forvarmes til 70°C. Denne vannholdige, findisperse faststoffsuspensjon homogeniseres med 35 vektdeler oppsmeltet bitumen B 80 i en knainnretning. Homogenisatet homogeniseres deretter med 56 vektdeler kalsiumoksyd som er blitt hydrofobert med 1% fettsyre. Det oppstår en med bitumen-homogent belastet, pulverformig faststoffsuspensjon som kan anvendes innenfor miljøbeskyttelsesområdet for isolering og for be-skyttelse av deponilegemer, samt til immobilisering av ikke-ionogene, uorganiske og også organiske skadelige stoffer. 56 parts by weight of clay are plasticized with 15 parts by weight of water and preheated to 70°C. This aqueous, finely dispersed solids suspension is homogenized with 35 parts by weight of melted bitumen B 80 in a kneader. The homogenize is then homogenized with 56 parts by weight of calcium oxide which has been hydrophobicized with 1% fatty acid. A bitumen-homogeneous laden, powdery solid suspension is created which can be used within the environmental protection area for insulation and for the protection of landfill bodies, as well as for the immobilization of non-ionic, inorganic and also organic harmful substances.
For dette formål blander man den eksempelvis i forholdet 1:4 med et kontaminert materiale som for eksempel inneholder halogenerte dibenzodioksiner, henholdsvis dibenzofuraner, i ppm-området. De eksakt nødvendige mengdeforhold fastslås ved enkle håndforsøk, idet opptakskapasiteten for det rene bitumen av den foreliggende type skadelig stoff og den skadelige stoffmengde bestemmes. For absorpsjon av skadelige stoffer med bestemte funksjonelle grupper blandes det opp-smeltede bitumen eksempelvis med den nødvendige mengde av et virksomt stoff som inneholder en funksjonell gruppe som er i stand til å reagere med det skadelige stoff, slik at adsorp-sjonslikevekten forskyves i retning mot en fullstendig absorpsjon. For behandling av skadelige stoffer som ikke lar seg immobilisere i alkalisk område, anvendes i stedet for kalsiumoksydet et aluminium-blandingsalkoholat av vanlig handelstype, for eksempel av aluminiumisopropanolat og aluminiumisobutanolat. I dette tilfelle er det spesielt fordelaktig dersom leiren erstattes med rødslam, ettersom dette findisperse system adsorberer de nevnte dioksiner og furaner spesielt godt i tørr tilstand. For this purpose, it is mixed, for example, in a ratio of 1:4 with a contaminated material which, for example, contains halogenated dibenzodioxins, respectively dibenzofurans, in the ppm range. The exact required quantity ratios are determined by simple hand tests, as the absorption capacity of the pure bitumen of the present type of harmful substance and the amount of harmful substance is determined. For the absorption of harmful substances with specific functional groups, the melted bitumen is mixed, for example, with the required amount of an active substance containing a functional group capable of reacting with the harmful substance, so that the adsorption equilibrium is shifted in the direction of a complete absorption. For the treatment of harmful substances which cannot be immobilized in an alkaline area, instead of the calcium oxide, an aluminum mixed alcoholate of the usual commercial type, for example of aluminum isopropanolate and aluminum isobutanolate, is used. In this case, it is particularly advantageous if the clay is replaced with red mud, as this finely dispersed system adsorbs the mentioned dioxins and furans particularly well in a dry state.
Eksempel 6 Example 6
150 vektdeler leire med et vanninnhold på 23% plastifiseres med 10 vektdeler vann i en knainnretning, og homogeniseres med 1 vektdel av et vannløselig salt av kobber, henholdsvis mangan, henholdsvis sink, henholdsvis molybden, henholdsvis bor, henholdsvis jern, for eksempel i form av de tilsvarende kobber-, jern-, mangan- og sinksulfater, henholdsvis som ammoniummolybdat, henholdsvis kaliummetaborat. Homogenisatene homogeniseres deretter med en jordalkalioksyd-blanding av 90% kalsiumoksyd og 10% magnesiumoksyd som er blitt hydrofobert med 0,2% fettsyre, i en knainnretning. De enkelte oppnådde homogene, pulverformige faststoffdispersjoner som er belastet med de angitte sporelementer, blandes i en fallrørblander i et mengdeforhold som tilsvarer den stilte oppgave. Man får et additiv for substratfremstilling av torv eller kompost. Additivets hydrofobe egenskaper fører til en hurtig blanding også med svært fuktig torv eller kompost. Når det her angis blandingsforhold som samsvarer med oppgavestillingen, så menes med dette det forskjellige behov som plantene har i sine forskjellige voksefaser. For det tilfelle at biotilgjengeligheten for enkelte komponenter skal forhøyes i overgjennomsnittlig grad, homogeniserer man leiren i den tilsvarende tilberedning i tillegg med 1 vektdel vinsyre eller for en ytterligere forhøyning av biotilgjengeligheten med 1 vektdel sitronsyre. 150 parts by weight of clay with a water content of 23% is plasticized with 10 parts by weight of water in a kneader, and homogenized with 1 part by weight of a water-soluble salt of copper, respectively manganese, respectively zinc, respectively molybdenum, respectively boron, respectively iron, for example in the form of the corresponding copper, iron, manganese and zinc sulphates, respectively as ammonium molybdate, respectively potassium metaborate. The homogenates are then homogenised with an alkaline earth oxide mixture of 90% calcium oxide and 10% magnesium oxide which has been hydrophobicized with 0.2% fatty acid, in a knave device. The individual obtained homogeneous, powdery solid dispersions loaded with the indicated trace elements are mixed in a downpipe mixer in a quantity ratio that corresponds to the task at hand. You get an additive for substrate production from peat or compost. The additive's hydrophobic properties lead to a rapid mixing even with very moist peat or compost. When mixing ratios are specified here that correspond to the task, this means the different needs that the plants have in their different growth phases. In the event that the bioavailability of certain components is to be increased to an above-average degree, the clay is homogenized in the corresponding preparation in addition with 1 part by weight of tartaric acid or for a further increase in bioavailability with 1 part by weight of citric acid.
Eksempel 7 Example 7
100 vektdeler leire eller slam (tysk: Lehm) plastifiseres med 10 vektdeler vann og homogeniseres med 2 0 vektdeler kalknitrogen; homogenisatet homogeniseres deretter med 10 vektdeler hydrofobt kalsiumoksyd. Den på denne måte oppnådde faststoffdispersjon kan anvendes for jordbruksformål som nitrogenholdig gjødningsmiddel med langtidsvirkning. 100 parts by weight of clay or silt (German: Lehm) is plasticized with 10 parts by weight of water and homogenized with 20 parts by weight of calcium nitrogen; the homogenise is then homogenised with 10 parts by weight of hydrophobic calcium oxide. The solid dispersion obtained in this way can be used for agricultural purposes as a nitrogen-containing fertilizer with a long-term effect.
Eksempel 8 Example 8
I en kombinasjon av eksemplene 2 og 5 homogeniseres In a combination of examples 2 and 5 homogenize
100 vektdeler leire med en suspensjon av 32 vektdeler jernsulfat i 7 vektdeler vann, med 8 vektdeler natriumsulfid og med 3 0 vektdeler oppsmeltet bitumen etter hverandre i en tvangsblander, og homogeniseres deretter med 28 vektdeler av et kalsiumoksyd som er hydrofobert med 0,5% fettsyre. Den pulverformige faststoffdispersjon som oppstår og som er homogent belastet med de virksomme stoffer jernsulfid og bitumen kan anvendes for samtidig irreversibel immobilisering av tungmetaller og ultragifter, for eksempel PCDD/DF i filterstøv og aske fra søppelforbrenningsanlegg, og som er kontaminert med slike stoffer. 100 parts by weight of clay with a suspension of 32 parts by weight of iron sulphate in 7 parts by weight of water, with 8 parts by weight of sodium sulphide and with 30 parts by weight of fused bitumen successively in a forced mixer, and then homogenised with 28 parts by weight of a calcium oxide hydrophobicized with 0.5% fatty acid . The resulting powdery solid dispersion, which is homogeneously loaded with the active substances iron sulphide and bitumen, can be used for the simultaneous irreversible immobilization of heavy metals and ultrapoisons, for example PCDD/DF in filter dust and ash from waste incineration plants, and which are contaminated with such substances.
Eksempel 9 Example 9
Et i hvert tilfelle to gangers overskudd av de støkio-metrisk nødvendige mengder av dikaliumhydrogenfosfat, jernsulfid og kalsiumkarbonat overføres i analogi med fremgang-småten i eksempel 1 hver for seg i homogene faststoffdispersjoner under anvendelse av kalsiumoksyd som er blitt hydrofobert med 1% fettsyre. Blandingen av de enkelte faststoffdispersjoner er fortreffelig egnet til irreversibel immobilisering av tungmetallioner i klaringsslam, komposter, elve- og havneslam, under utfelling av de enkelte tungmetaller som karbonater, sulfider og fosfater. Også arsen og antimon lar seg fiksere kjemisk på denne måte. Til dette formål blander man de nevnte faststoffdispersjoner samtidig med ytterligere, svakt hydrofobert kalsiumoksyd inn i de avfallsstoffer som skal behandles, for eksempel ved synkron tilførsel i en fall-rørblander. På denne måte blir det for første gang mulig å lagre store mengder av disse avfallsstoffer uten ytterligere sikringstiltak på miljønøytral måte eller anvende disse stoffer som jordbygningsstoff, for eksempel for landskapsopp-byggingsformål. De mengdeforhold som kreves bestemmes av grunnens mekaniske krav; de lar seg bestemme ved de kjente egnethetsbestemmelser, for eksempel ved bestemmelse av proktordensitet. In each case, a two-fold excess of the stoichiometrically required quantities of dipotassium hydrogen phosphate, iron sulphide and calcium carbonate is transferred in analogy to the procedure in example 1 separately in homogeneous solid dispersions using calcium oxide which has been hydrophobicized with 1% fatty acid. The mixture of the individual solid dispersions is excellently suited for the irreversible immobilization of heavy metal ions in sewage sludge, composts, river and harbor sludge, during precipitation of the individual heavy metals such as carbonates, sulphides and phosphates. Arsenic and antimony can also be fixed chemically in this way. For this purpose, the aforementioned solid dispersions are simultaneously mixed with additional, weakly hydrophobic calcium oxide into the waste materials to be treated, for example by synchronous feeding in a downpipe mixer. In this way, it will be possible for the first time to store large quantities of these waste substances without further safeguards in an environmentally neutral way or to use these substances as soil building material, for example for landscaping purposes. The quantity ratios required are determined by the mechanical requirements of the soil; they can be determined by the known suitability determinations, for example by determining proctor density.
Eksempel 10 Example 10
100 vektdeler leire eller findisperst aluminiumhydroksyd eller zeolitt eller bentonitt som er bearbeidet til en deig med vann, eller brukt, fuktig blekejord, eller 100 vektdeler av en blanding av de nevnte faststoffsuspensjoner homogeniseres med 50 vektdeler av et langkjedet amin, for eksempel stearylamin, og 10 vektdeler av et aminosilan, for eksempel et trialkoksyaminosilan, homogeniseres i en knainnretning og homogeniseres deretter med 500 vektdeler hydrofobt kalsiumoksyd. Den tørre, pulverformige og homogene faststoffdispersjon som oppstår og som inneholder et overskudd av kalsiumoksyd, lar seg anvende som sådan eller etter forløp av hydratasjonsreaksjonen med ikke fullstendig den støkio-metriske nødvendige vannmengde i forhold til kalsiumoksyd-overskuddet, i form av følgeproduktet, dvs. med kalsiumhydroksyd som mengdemessig overveiende komponent, til den mest vidtgående absorpsjon, henholdsvis kjemisorpsjon, av skadelige stoffer i avgasser fra søppelforbrenningsanlegg, spesielt av halogenerte dibenzodioksiner og dibenzofuraner. 100 parts by weight of clay or finely dispersed aluminum hydroxide or zeolite or bentonite which has been worked into a dough with water, or used moist bleaching earth, or 100 parts by weight of a mixture of the aforementioned solid suspensions are homogenized with 50 parts by weight of a long-chain amine, for example stearylamine, and 10 parts by weight of an aminosilane, for example a trialkoxyaminosilane, are homogenized in a kneading device and then homogenized with 500 parts by weight of hydrophobic calcium oxide. The dry, powdery and homogeneous solid dispersion that occurs and which contains an excess of calcium oxide can be used as such or after the course of the hydration reaction with not quite the stoichiometric required amount of water in relation to the calcium oxide excess, in the form of the by-product, i.e. with calcium hydroxide as the quantitatively predominant component, for the most extensive absorption, respectively chemisorption, of harmful substances in waste gases from waste incineration plants, especially of halogenated dibenzodioxins and dibenzofurans.
Eksempel 11 Example 11
100 vektdeler leire eller findisperst aluminiumhydroksyd eller zeolitt eller bentonitt som med vann er bearbeidet til en deig, eller brukt, fuktig blekejord, eller 100 vektdeler av en blanding av de nevnte faststoffsuspensjoner ble homogenisert med 50 vektdeler av et alkali-' eller jordalkali-sulfid i en knainnretning, og deretter homogenisert med 150 vektdeler hydrofobt kalsiumoksyd. Den tørre, pulverformige og homogene faststoffdispersjon som oppstår, og som inneholder et overskudd av kalsiumoksyd, lar seg på grunn av den hydrofobe karakter lett innarbeide i overflaten av av-fallshauger som består av tungmetallholdige produksjonsrester. På denne måte oppstår et flatdekkende depot med utfellingsreagenser som på grunn av langsomt forløpende desorpsjonsprosesser (sulfidioner), henholdsvis på grunn av den tunge løselighet (kalsiumhydroksyd og kalsiumkarbonat av kalsiumoksyd), bare svært langsomt føres inn i haugen med regnvannet som bærer og der fører til utfellingsreaksjoner in situ. De for dette formål nødvendige absolutte mengder av 100 parts by weight of clay or finely dispersed aluminum hydroxide or zeolite or bentonite which has been processed with water into a dough, or used moist bleaching earth, or 100 parts by weight of a mixture of the aforementioned solid suspensions were homogenized with 50 parts by weight of an alkali or alkaline earth sulphide in a kneading device, and then homogenized with 150 parts by weight of hydrophobic calcium oxide. The resulting dry, powdery and homogeneous solid dispersion, which contains an excess of calcium oxide, can easily be incorporated into the surface of waste piles consisting of heavy metal-containing production residues due to its hydrophobic nature. In this way, a flat-covering deposit is created with precipitation reagents which, due to slow desorption processes (sulphide ions), respectively due to the heavy solubility (calcium hydroxide and calcium carbonate of calcium oxide), are only very slowly introduced into the heap with the rainwater as a carrier and there lead to precipitation reactions in situ. The necessary absolute quantities of for this purpose
utfellingsreagenser og dermed depotets sjikttykkelse lar seg lett bestemme ut fra haugens høyde og den midlere konsentrasjon av utfellbare tungmetaller i haugen. Man går frem på analogt vis for immobilisering av skadelige stoffer i andre påfylte lagringsplasser og deponier. precipitation reagents and thus the deposit's layer thickness can be easily determined from the height of the pile and the average concentration of precipitable heavy metals in the pile. The process is analogous to the immobilization of harmful substances in other filled storage areas and landfills.
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DE4106515A DE4106515C2 (en) | 1991-03-01 | 1991-03-01 | Process for the production of a powdery, finely disperse dispersion homogeneously loaded with active ingredients and the use of products obtained thereafter |
DE19914106516 DE4106516C2 (en) | 1991-03-01 | 1991-03-01 | Process for producing a powdery, homogeneous, finely dispersed dispersion and the use of products obtained therefrom |
PCT/EP1992/000436 WO1992015539A1 (en) | 1991-03-01 | 1992-02-28 | Method for producing homogeneous, fine, pulverulent solids dispersions optionally containing active substances |
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JP (1) | JPH05507440A (en) |
KR (1) | KR100220560B1 (en) |
AU (1) | AU648391B2 (en) |
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DE2533791C3 (en) * | 1975-07-29 | 1981-06-19 | Bölsing, Friedrich, Prof. Dr. Dipl.-Chem., 3067 Lindhorst | Process for the production of solid and / or liquid substances or mixtures of substances in finely divided solid hydroxides |
DE3632365A1 (en) * | 1986-09-24 | 1988-03-31 | Friedrich Boelsing | METHOD FOR IMMOBILIZING POLLUTANTS IN THE FLOOR OR FLOOR-LIKE MATERIALS |
DE3632363A1 (en) * | 1986-09-24 | 1988-03-31 | Boelsing Friedrich | METHOD FOR DEHALOGENATING HALOGENED CARBON HYDROGEN |
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- 1992-02-28 KR KR1019920702715A patent/KR100220560B1/en not_active IP Right Cessation
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NO924190D0 (en) | 1992-10-30 |
CA2081307A1 (en) | 1992-09-02 |
JPH05507440A (en) | 1993-10-28 |
NO924190L (en) | 1992-10-30 |
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