EP0507895A1 - Verfahren zur herstellung von einem spherosilikatzement und daraus hergestellter zement - Google Patents
Verfahren zur herstellung von einem spherosilikatzement und daraus hergestellter zementInfo
- Publication number
- EP0507895A1 EP0507895A1 EP91914369A EP91914369A EP0507895A1 EP 0507895 A1 EP0507895 A1 EP 0507895A1 EP 91914369 A EP91914369 A EP 91914369A EP 91914369 A EP91914369 A EP 91914369A EP 0507895 A1 EP0507895 A1 EP 0507895A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- sio
- parts
- spherosilicate
- silicate
- equal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- 239000004568 cement Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims description 12
- 239000011575 calcium Substances 0.000 claims abstract description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000011230 binding agent Substances 0.000 claims abstract description 34
- 238000005481 NMR spectroscopy Methods 0.000 claims abstract description 25
- 239000011734 sodium Substances 0.000 claims abstract description 21
- 229910052918 calcium silicate Inorganic materials 0.000 claims abstract description 19
- 239000000378 calcium silicate Substances 0.000 claims abstract description 18
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 claims abstract description 18
- 150000001768 cations Chemical class 0.000 claims abstract description 18
- 238000004458 analytical method Methods 0.000 claims abstract description 15
- 229910000323 aluminium silicate Inorganic materials 0.000 claims abstract description 12
- 238000001228 spectrum Methods 0.000 claims abstract description 12
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 9
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 8
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 8
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910001424 calcium ion Inorganic materials 0.000 claims abstract description 6
- 239000011591 potassium Substances 0.000 claims abstract description 6
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims abstract description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 83
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 69
- 239000000203 mixture Substances 0.000 claims description 65
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 36
- 239000011707 mineral Substances 0.000 claims description 36
- 235000010755 mineral Nutrition 0.000 claims description 36
- 239000002893 slag Substances 0.000 claims description 26
- 238000006068 polycondensation reaction Methods 0.000 claims description 22
- 235000012241 calcium silicate Nutrition 0.000 claims description 20
- 239000004570 mortar (masonry) Substances 0.000 claims description 16
- 239000004111 Potassium silicate Substances 0.000 claims description 15
- 229910052913 potassium silicate Inorganic materials 0.000 claims description 15
- 235000019353 potassium silicate Nutrition 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 15
- UFFNHUYHCDHKHK-UHFFFAOYSA-N hexapotassium trioxido(trioxidosilyloxy)silane Chemical group [K+].[K+].[K+].[K+].[K+].[K+].[O-][Si]([O-])([O-])O[Si]([O-])([O-])[O-] UFFNHUYHCDHKHK-UHFFFAOYSA-N 0.000 claims description 14
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 13
- 229910001678 gehlenite Inorganic materials 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 239000004576 sand Substances 0.000 claims description 10
- 230000015572 biosynthetic process Effects 0.000 claims description 9
- 229910052882 wollastonite Inorganic materials 0.000 claims description 8
- 239000010456 wollastonite Substances 0.000 claims description 8
- 229910001720 Åkermanite Inorganic materials 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 7
- 238000000655 nuclear magnetic resonance spectrum Methods 0.000 claims description 6
- 239000000945 filler Substances 0.000 claims description 5
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 claims description 3
- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical compound [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 claims description 3
- 239000010881 fly ash Substances 0.000 claims description 3
- PMYUVOOOQDGQNW-UHFFFAOYSA-N hexasodium;trioxido(trioxidosilyloxy)silane Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[O-][Si]([O-])([O-])O[Si]([O-])([O-])[O-] PMYUVOOOQDGQNW-UHFFFAOYSA-N 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 238000006116 polymerization reaction Methods 0.000 claims description 3
- 235000012215 calcium aluminium silicate Nutrition 0.000 claims description 2
- BCAARMUWIRURQS-UHFFFAOYSA-N dicalcium;oxocalcium;silicate Chemical compound [Ca+2].[Ca+2].[Ca]=O.[O-][Si]([O-])([O-])[O-] BCAARMUWIRURQS-UHFFFAOYSA-N 0.000 claims description 2
- MKTRXTLKNXLULX-UHFFFAOYSA-P pentacalcium;dioxido(oxo)silane;hydron;tetrahydrate Chemical compound [H+].[H+].O.O.O.O.[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O MKTRXTLKNXLULX-UHFFFAOYSA-P 0.000 claims description 2
- 235000019976 tricalcium silicate Nutrition 0.000 claims description 2
- 229910021534 tricalcium silicate Inorganic materials 0.000 claims description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims 2
- 235000015076 Shorea robusta Nutrition 0.000 claims 1
- 244000166071 Shorea robusta Species 0.000 claims 1
- 239000000404 calcium aluminium silicate Substances 0.000 claims 1
- WNCYAPRTYDMSFP-UHFFFAOYSA-N calcium aluminosilicate Chemical compound [Al+3].[Al+3].[Ca+2].[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O WNCYAPRTYDMSFP-UHFFFAOYSA-N 0.000 claims 1
- 229940078583 calcium aluminosilicate Drugs 0.000 claims 1
- 229910000019 calcium carbonate Inorganic materials 0.000 claims 1
- JHLNERQLKQQLRZ-UHFFFAOYSA-N calcium silicate Chemical compound [Ca+2].[Ca+2].[O-][Si]([O-])([O-])[O-] JHLNERQLKQQLRZ-UHFFFAOYSA-N 0.000 claims 1
- 238000010952 in-situ formation Methods 0.000 claims 1
- 239000006104 solid solution Substances 0.000 claims 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 4
- 229910052593 corundum Inorganic materials 0.000 abstract 4
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 4
- 235000011118 potassium hydroxide Nutrition 0.000 description 26
- 239000000377 silicon dioxide Substances 0.000 description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 21
- 239000000779 smoke Substances 0.000 description 16
- 229910004298 SiO 2 Inorganic materials 0.000 description 15
- 150000004760 silicates Chemical class 0.000 description 14
- 239000008267 milk Substances 0.000 description 12
- 235000013336 milk Nutrition 0.000 description 12
- 210000004080 milk Anatomy 0.000 description 12
- 239000003153 chemical reaction reagent Substances 0.000 description 11
- FZVXUPLDQNBUQZ-UHFFFAOYSA-N [Ca+2].[Ca+2].[Ca+2].[O-][Si]([O-])([O-])O[Si]([O-])([O-])[O-] Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-][Si]([O-])([O-])O[Si]([O-])([O-])[O-] FZVXUPLDQNBUQZ-UHFFFAOYSA-N 0.000 description 9
- 229910052791 calcium Inorganic materials 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical group [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 8
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical group [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 8
- 235000011121 sodium hydroxide Nutrition 0.000 description 8
- 239000007788 liquid Substances 0.000 description 7
- -1 calcium aluminates Chemical class 0.000 description 6
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000009471 action Effects 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 4
- 230000036571 hydration Effects 0.000 description 4
- 238000006703 hydration reaction Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 230000006835 compression Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- 239000005909 Kieselgur Substances 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 239000011398 Portland cement Substances 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- BFRXZIMAUMUZJH-UHFFFAOYSA-M [OH-].[Na+].[Na+].[Na+].[Na+].[Al+3].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] Chemical compound [OH-].[Na+].[Na+].[Na+].[Na+].[Al+3].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] BFRXZIMAUMUZJH-UHFFFAOYSA-M 0.000 description 2
- 229910052910 alkali metal silicate Inorganic materials 0.000 description 2
- 239000002956 ash Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000004567 concrete Substances 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000004455 differential thermal analysis Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000003517 fume Substances 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 159000000011 group IA salts Chemical class 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000002440 industrial waste Substances 0.000 description 2
- 229910052622 kaolinite Inorganic materials 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 235000011181 potassium carbonates Nutrition 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 239000012429 reaction media Substances 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 229910021487 silica fume Inorganic materials 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- 238000007725 thermal activation Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910004283 SiO 4 Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000001994 activation Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910001854 alkali hydroxide Inorganic materials 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 229910001583 allophane Inorganic materials 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 235000013365 dairy product Nutrition 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 150000004673 fluoride salts Chemical class 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000011396 hydraulic cement Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910052900 illite Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- BHGADZKHWXCHKX-UHFFFAOYSA-N methane;potassium Chemical compound C.[K] BHGADZKHWXCHKX-UHFFFAOYSA-N 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- VGIBGUSAECPPNB-UHFFFAOYSA-L nonaaluminum;magnesium;tripotassium;1,3-dioxido-2,4,5-trioxa-1,3-disilabicyclo[1.1.1]pentane;iron(2+);oxygen(2-);fluoride;hydroxide Chemical compound [OH-].[O-2].[O-2].[O-2].[O-2].[O-2].[F-].[Mg+2].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[K+].[K+].[K+].[Fe+2].O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2 VGIBGUSAECPPNB-UHFFFAOYSA-L 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229940072033 potash Drugs 0.000 description 1
- 235000015320 potassium carbonate Nutrition 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical class [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- BHZRJJOHZFYXTO-UHFFFAOYSA-L potassium sulfite Chemical class [K+].[K+].[O-]S([O-])=O BHZRJJOHZFYXTO-UHFFFAOYSA-L 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 235000019252 potassium sulphite Nutrition 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 235000011182 sodium carbonates Nutrition 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 230000007928 solubilization Effects 0.000 description 1
- 238000005063 solubilization Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical class [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000005335 volcanic glass Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B12/00—Cements not provided for in groups C04B7/00 - C04B11/00
- C04B12/005—Geopolymer cements, e.g. reaction products of aluminosilicates with alkali metal hydroxides or silicates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/006—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing mineral polymers, e.g. geopolymers of the Davidovits type
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Definitions
- the present invention relates to a process for preparing a cement of the spherosilicate type which hardens quickly at room temperature, as well as the cement obtained by this process. More specifically, the mineral compositions described in the invention make it possible to obtain a cement of the spherosilicate type having a setting time equal to or greater than 30 minutes at the temperature of 20 ° C. and a curing speed making it possible to obtain resistances at compression (Rc) equal to or greater than 15 MPa, after only U hours at 20 C, when tested according to the standard standard applied to hydraulic binder mortars with a binder / sand ratio equal to 0.38 and a ratio water / binder between 0.22 and 0.27.
- Rc resistances at compression
- the mineral compositions of the spherosilicate type according to the present invention making it possible to obtain a cement of the spherosilicate type with rapid hardening, (Rc)> 15 MPa at 4 h - 20 C, essentially comprise three reactive elements.
- the first reagent is an aluminum silicate oxide (2SiO_, ALO_) having the cation Al in coordination (IV-V) as determined by the analysis spectrum of Nuclear Magnetic Resonance MASS-NMR
- this alumino-silicate oxide (2Si0 2 , ALO-) is obtained by heat treatment, in an oxidizing medium, of natural hydrated alumino-silicates, in which the cation Al is in coordination (VI) as determined by the spectrum Resonance analysis
- the second reagent is a sodium and / or potassium disilicate, soluble in water, (Na 2 , K_) (H_SiO ⁇ ) 2 ; potassium disilicate K 2 (H 3 SiO 2 ) 2 will preferably be used although the sodium disilicate Na- (H, SiO 2 ) 2 also makes it possible to produce mineral compositions of the spherosilicate type according to the invention. It is also possible to use a mixture of the two alkaline disilicates.
- the third reagent is a basic calcium silicate, that is to say with a Ca / Si atomic ratio equal to or greater than 1. It will be essentially characterized by its ability to generate, under the action of an alkaline attack, the formation of weakly basic calcium silicate, that is to say having a Ca / Si atomic ratio of less than 1, preferably close to 0 , 5. This characterization will be established using X-ray Photoelectron Spectrometry (X.p. s.) And by analysis of the Ca_ / Si- relationships as indicated by M. Regourd, Phil. Trans. Royal Society London, A.310, pages 85-92 (1983).
- the mineral compositions of the invention are also called mineral compositions of the spherosilicate type, since the cement of the spherosilicate type obtained results from a mineral polycondensation reaction as opposed to traditional hydraulic binders in which hardening is the result of hydration of calcium aluminates and calcium silicates.
- the means of investigation used is the Magnetic Resonance spectrum
- the fast-curing mineral binder, (Rc) 15 MPa at 4h - 20 ° C corresponds to a material of the spherosilicate type of the type (Ca, K) -poIy (sialate-siIoxo) of formula varying between
- Binders and cements having rapid hardening and based on reactions of the mineral polycondensation type involving the three reagents used in the present invention have been proposed in the past.
- This composition comprises 840 g of a so-called "standard" reaction mixture to which has been added, in addition to inert fillers, 220 g of ground blast furnace slag.
- the reaction components of the spherosilicate type are characterized by the molar ratios of the oxides:
- composition of the spherosilicate type comprising 1 mole of the oxide alumino-silicate (2SiO 2 , ALO 3 ), i.e. 222 g, 1.12 moles of potassium disilicate K 2 (H 3 SiO _, or 300 g, 0.21 moles K 2 0 corresponding to 28 g of anhydrous KOH at 90 I, and 290 g of water and 220 g of slag.
- the mineral compositions of the spherosilicate type are characterized by the molar ratios between the three reactive elements which are equal or between
- the amount of alkaline disilicate is reduced from 200% to 300% compared to the prior state of the art. It was not enough, for this, to simply lower the amount of this alkaline disilicate. Indeed, it was surprising to note that it was essentially necessary to change the physical state of the constituents.
- the aforementioned known compositions are in the liquid phase.
- the slag is added to an aqueous reaction mixture containing the aluminum silicate oxide (2SiO 2 , ALO 2 ), the alkalis, the water and the potassium polysilicate in solution.
- the mineral compositions of the spherosilicate type are in the solid phase, in particular the second reagent, the sodium and / or potassium disilicate (Na 2 , K 2 ) (f-SiO. is a finely divided powder, water being added only in the final phase of mixing the mortar or binder.
- mineral powder compositions for example mineral compositions comprising:
- amorphous silica In this latter composition, the role of amorphous silica is essentially to replace part of the potassium silicate necessary for mineral polycondensation, that is to say that the amorphous silica reacts with potassium hydroxide to produce, in the mortar, the quantity of potassium silicate desired.
- potassium silicate means industrial potassium silicate, in powder form, corresponding to the formula K 2 O, 3SiO 2 , 3H 2 O, soluble in water and making it possible to produce binders and adhesives having the same properties as "soluble glasses” or alkali silicate in solution.
- the compressive strength Rc at 4 h - 23 C is only around 6.9 MPa, which is much lower than (Rc)> 15 MPa at 4 h - 20 ° C, as claimed in the present invention.
- Rc at 4 h - 23 C is only about 4.6 MPa, while in still other examples, only Rc at around 65 C are given, Rc at 4 - 23 C being too weak to be mentioned.
- the powdered alkaline disilicate makes it possible to obtain a cement of the spherosilicate type having a rapid hardening, at 20 ° C., in a few hours, i.e. (Rc)> 15 MPa at 4h - 20 ° C.
- the mineral composition of the spherosilicate type comprises for 52 parts of metakaolin, 24 to 28 parts of potassium hydroxide, 73 to 120 parts of silica smoke, 18 to 29 parts of slag.
- Silica smoke reacts with potassium hydroxide to produce potassium silicate in the mixture, which is a way of lowering the cost price of this very expensive reagent.
- K 2 (H 3 SiO) 2 from 0.215 to 0.25 moles which gives a ratio K j on (2SiO 2 , ALO_) between 0.93 and 1.08, again practically the ratios discussed above.
- mixture A oxide (2Si0 2 , AL0 3 ) 400 g micronized mica 100 g
- mixture B oxide (2Si0 2 A! 2 0 3 ) 400 g silica smoke 100 g
- liquid 1 40% potassium silicate solution 520 g
- liquid 2 40% sodium silicate solution 1040 g
- the mixture between the powder and the liquid is carried out according to the pro ⁇ portions indicated in the table, and the mineral polycondensation is followed by Differential Thermal Analysis.
- the values of the J / g ratio are compared, that is to say the amount of energy measured in Joules on the weight of the sample in grams.
- the mineral polycondensation temperature is 60 C.
- test No. 2 (with silica smoke) is divided by 5 compared to that of test No. 1 (without silica smoke), and that of test No. 3 is divided by 2.
- amorphous silica such as silica fume or other silicas which it is known that they can easily transform into potassium or sodium silicate, at moderate or even ambient temperature, will be added in such a quantity that it will not disturb the natural exothermicity of the mixture of the spherosilicate type.
- Amorphous silica such as, for example, silica smoke, rice ash, diatomaceous earth, silicic smectites, certain strongly silicic pozzolans (with a high percentage of allophane and glass of volcanic origin) are considered as finely divided, reactive loads.
- the third reagent of the invention is weakly basic calcium silicate with the Ca / Si atomic ratio of less than 1.
- This third reagent is linked to the preceding ones by the molar ratios between the three reactive elements equal to or comprised between
- the sum of the number of moles of calcium disilicate, Ca (H, SiO y ) _, and the number of moles of potassium disilicate, K_ (H, SiO y ) _, is equal to the number of moles of the aluminum silicate oxide (2SiO_, ALO_).
- This alumino-silicate oxide (2Si0 2 , AL0 3 ) determines all the reaction conditions of the mineral compositions of the spherosilicate type. It will react with an alkaline or alkaline earth disilicate to form, after mineral polycondensation, a compound (Si 2 O_, ALO 2 , Si 2 O 5 , (K 2 O, CaO)), i.e. (K, Ca) -poly (sialate-siloxo) of formula between
- the oxide (2Si0 2 , AL0 3 ) reacts first with the most soluble disilicate which is always the alkaline disilicate (Na 2 , K 2 ) (H 3 SiO.) 2 .
- the amount of calcium dislicate involved in the mineral polycondensation reaction is essentially determined by the amount of alkaline disilicate. If the sum of the moles of these disilicates is greater than 1, the non-reacting part will be that which is the least soluble, that is to say the calcium disilicate.
- Calcium disilicate Ca (H_SiO i .) 2 can be produced separately, for example by hydrothermal reaction between lime and silica.
- the starting material is a basic calcium silicate, that is to say with the Ca / Si atomic ratio greater than or equal to 1.
- This will be for example wollastonite Ca (Si0 3 ), gehlenite (2CaO .AI 2 0 3. Si0 2 ), bicalcium silicate C 2 S (2CaO.Si0 2 ), tricalcium silicate CS (3CaO .Si0 2 ), Akermanite (2CaO.SiO 2 ).
- Blast furnace slag essentially contains the basic silicates gehlenite, akermanite, wollastonite and is therefore very suitable.
- This process is very regular and can be completed in 30 minutes, at room temperature.
- C 2 S there occurs in a few seconds a high concentration of weakly basic silicate Ca / Si less than 1; then the attack is stopped, and then continues more regularly. This is called the "flash-set" or formation of a gel creating a false catch.
- setting retarders like those commonly used in cement mixtures portiand.
- the mineral polycondensation reaction used in the present invention should not be confused with the simple alkaline activation of hydraulic binders, or with the action of alkali setting accelerator on portland cements and other hydraulic binders. Indeed, the simple action of alkalis, NaOH or KOH, on portland cements or blast furnace slag, results in the production of hydrated calcium silicates, as mentioned above. In contrast to what happens in the present invention, these hydrated silicates crystallize to form CSH, the main constituent of hydraulic calcium cements.
- the CSH is a monosilicate and / or a bisilicate, that is to say that the SiO 2 tetrahedra which constitute it belong to the category (QO), (Ql) and possibly (Q2).
- the mineral polycondensation leads to the formation of SiO tetraera of type (Q4, as determined by the analysis spectrum in Nuclear Magnetic Resonance MASS-NMR for 29 Si.
- alkalis, NaOH and KOH are setting accelerators, they do not constitute hardening accelerators capable of achieving the object of the invention, that is to say (Rc) 15 MPa at 4 h - 20 ° C .
- the hardening accelerator is usually temperature or the addition of portiand cement. It is for example known to use a cement based on slag, portian cement or lime, and an alkaline accelerator such as NaOH and sodium and or potassium carbonates.
- a mixture comprising alumino-silicate oxide (2Si0 2 , AL0 3 ), slag (or cement) and alkalies KOH, NaOH, does not constitute a mineral binder of mineral polycondensation according to the present invention. It is known that a mortar made with this mixture and water does not harden at 20 C for 24 hours. Thus it is known that if the oxide (2Si0 2 , ALO_) is not masked by a polysilicate solution against the attack of strong bases KOH, NaOH, a simple poly (sialate) of the type is formed. hydroxysodalite and which precipitates without binding function. It is known that hydroxysodalite constitutes a binder only in ceramic pastes, with very little water and when the material is compressed.
- the third reagent of the mineral polycondensation composition is calcium silicate. It can be accompanied by complex calcium aluminates and silicates.
- blast furnace slag is partly formed of a glass composed inter alia of gehlenite 2CaO.AL0 3 .Si0 2 , of akermanite 2Ca0.Mg0.2Si0 2 , of wollastonite.
- AI (V1) equal to or greater than 1.
- SiO j (Q) is 4 to 6 times greater than the sum of the concentrations of SiO tetrahedrons ask(QO) + (Q1) + (Q2), and depending on the nature of the charges we will have
- Blast furnace slag is a cheap source of wollastonite, gehlenite and ackermanite.
- the mineral polycondensation compositions of the invention containing blast furnace slag make it possible to produce a mineral polycondensation binder, in powder form, containing: a) 100 parts by weight of aluminum silicate oxide (2SiO-, ALO,) having the cation Al in coordination
- the mortar obtained by adding a quantity of water such that the water / binder ratio is between 0.20 and 0.27 and a quantity of standardized sand such that the binder / sand ratio 0.38 hardens cold and develops after 4 hours at 20 ° C a compressive strength greater than or equal to 15 MPa.
- setting is considered to be slow, since it takes place after a time of more than 30 minutes without the addition of retarder, which allows use in industry, with traditional mixers .
- retarder which allows use in industry, with traditional mixers .
- the table groups the setting times for different milk / water weight ratios, compositions involving alkali silicate solutions and inorganic polycondensation compositions containing powdered alkaline disilicates, according to the present invention.
- start of setting (at 20 ° C.) for the present invention 30 min 60 min 90 min 3 hours
- potassium disilicate K 2 H., SiO 2
- sodium disilicate Na 2 H, SiO tt _
- sources of impure alkalis containing both potassium and sodium This is often the case for industrial waste very rich in alkalis such as filter dust from portain cement calcining furnaces or alkaline detergents from the mining industry or chemical.
- the advantage of the present invention also lies in the fact that the use of alkaline disilicate (Na 2 , K 2 ) (H 3 SiO 2 ) 2 in powder makes it possible to use inexpensive raw materials coming from industrial waste.
- An interesting source of amorphous silica is the silica smoke recovered in the filters above the melting furnaces of ferro-silicone steels. These silica fumes contain 90-95% Si0 2 , carbon, and 0.5-1% finely dispersed metallic silicon. These silica fumes make it possible to manufacture the alkaline disilicate at very low temperatures, even at ordinary temperature.
- silica sands it is generally necessary to work in an autoclave when reacting alkali hydroxides, or in fusion when using alkali carbonates. It is also possible to use amorphous silica of natural origin such as diatomaceous earth, very siliceous smectics and gaizes, very siliceous volcanic glasses and pozzolans. Ash rich in silica, obtained by calcining plants (rice for example), can also be used for this purpose.
- the manufacture of aluminum silicate oxide (2SiO 2 , ALO,) is carried out by treating between 650 ° C and 800 ° C kaolinitic clays.
- Kaolinitic sands can be used as raw material, as well as certain clays containing at the same time kaolinite, montmorillonite and illite; likewise lateritic soils and laterites containing both kaolinite. Tests carried out on pyrophillites show that these materials are suitable for mineral polycondensation.
- the heat treatment temperatures of the raw materials must be adjusted so that they allow optimum production of aluminum silicate oxide (2SiO 2 , AO 3 ) having the highest concentration of Al coordinating Al (IV-V) as
- the alkalis are generally the sodium and / or potassium hydroxides produced industrially by electrolysis. They are also the result of the chemical reaction between an alkaline salt and calcium hydroxide or a material producing it in situ.
- the alkaline salts are selected from sodium and potassium carbonates, potassium sulfates, potassium sulfites. It is thus possible to use the dust collected on the filters of portiand cement kilns which are very rich in sulfites and sulfates. potassium, convert them to carbonates using the Leblanc process, or react them with clinker to produce potassium hydroxide in situ.
- the powdered alkaline disilicates obtained in this case during the reaction between the amorphous silicas and the alkalis as in Example 1 below are rather double potassium and calcium disilicates. They also allow the present invention to be carried out.
- the molar ratio K 2 (H 3 SiO.) 2 / (2Si0 2 , AL0 3 ) is equal to 0.43.
- the dairy / alkaline disilicate weight ratio is equal to
- a mortar is made as in example 2.
- the molar ratio K 2 (H 3 SiO 2 / (2Si0 2 , ALO,) is equal to 0.56.
- the milk / alkaline disilicate weight ratio is equal to
- Example 2 22 parts of (2Si0 2 , AL0 3 ), 15 parts of slag, 20 parts of silica smoke and 11 parts of KOH are mixed dry, then the sand is added and then 25 parts of water. A mortar is thus obtained as in Example 2. There is no setting, even at 24 hours at 20 ° C.
- a mixture containing 27 parts of (2SiO 2 , ALO_), 21 parts of slag, 15 parts of fumed silica and 19 parts of potassium disilicate K 2 (H 3 SiO 2 prepared according to Example 1) is prepared dry. 215 parts of standardized sand and then 21.5 parts of water.
- the starts after 35 minutes, and the resistance Rc after 4 hours at 20 ° C is 16 MPa, with a water / binder ratio 0.26.
- the molar ratio K 2 (H 3 SiO 2 is equal to 0.58.
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EP (1) | EP0507895A1 (de) |
AU (1) | AU8422591A (de) |
CS (1) | CS270091A3 (de) |
EC (1) | ECSP910776A (de) |
ES (1) | ES2033584B1 (de) |
GB (1) | GB2247453A (de) |
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CH682561A5 (de) * | 1990-09-03 | 1993-10-15 | Holderbank Financ Glarus | Tectoalumosilicat-Zement, daraus erhaltene Bindemittelmatrix, und Beton mit dieser Bindemittelmatrix. |
BR0114402A (pt) * | 2000-10-05 | 2003-07-29 | Suz-Chung Ko | Cimento de escórias |
FR2882276A1 (fr) * | 2005-02-21 | 2006-08-25 | Philippe Pichat | Fabrication d'un materiau solide a partir d'un hydroxyde alcalin |
WO2007109862A1 (en) | 2006-03-29 | 2007-10-04 | Zeobond Research Pty Ltd | Dry mix cement composition, methods and systems involving same |
FR2904972B1 (fr) * | 2006-08-21 | 2009-12-18 | Philippe Pichat | Composition a prise hydraulique. |
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DE3071695D1 (en) * | 1979-09-04 | 1986-09-18 | Joseph Davidovits | Synthetic inorganic polymer of the silicoaluminate family and process for the preparation thereof; moulded articles containing this polymer, and process for their preparation |
US4509985A (en) * | 1984-02-22 | 1985-04-09 | Pyrament Inc. | Early high-strength mineral polymer |
US4642137A (en) * | 1985-03-06 | 1987-02-10 | Lone Star Industries, Inc. | Mineral binder and compositions employing the same |
US4640715A (en) * | 1985-03-06 | 1987-02-03 | Lone Star Industries, Inc. | Mineral binder and compositions employing the same |
WO1988002741A1 (fr) * | 1986-10-14 | 1988-04-21 | Nicolas Davidovits | Materiau composite ceramique-ceramique et procede d'obtention |
FR2657867B1 (fr) * | 1990-02-05 | 1994-01-14 | Joseph Davidovits | Ciment rapide geopolymerique a base de ciment portland et procede d'obtention. |
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- 1991-08-24 EP EP91914369A patent/EP0507895A1/de not_active Withdrawn
- 1991-08-24 WO PCT/EP1991/001608 patent/WO1992004295A1/fr not_active Application Discontinuation
- 1991-08-24 AU AU84225/91A patent/AU8422591A/en not_active Abandoned
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- 1991-09-02 EC ECSP910776 patent/ECSP910776A/es unknown
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ES2033584A1 (es) | 1993-03-16 |
GB2247453A (en) | 1992-03-04 |
AU8422591A (en) | 1992-03-30 |
GB9118639D0 (en) | 1991-10-16 |
WO1992004295A1 (fr) | 1992-03-19 |
WO1992004294A1 (fr) | 1992-03-19 |
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