GB2401103A - Synthetic magnesium silicate compositions, methods and uses - Google Patents
Synthetic magnesium silicate compositions, methods and uses Download PDFInfo
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- GB2401103A GB2401103A GB0309620A GB0309620A GB2401103A GB 2401103 A GB2401103 A GB 2401103A GB 0309620 A GB0309620 A GB 0309620A GB 0309620 A GB0309620 A GB 0309620A GB 2401103 A GB2401103 A GB 2401103A
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- composition
- magnesium silicate
- synthetic magnesium
- formula
- hydrated
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- 239000000203 mixture Substances 0.000 title claims abstract description 118
- XCOBTUNSZUJCDH-UHFFFAOYSA-B lithium magnesium sodium silicate Chemical compound [Li+].[Li+].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Na+].[Na+].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3 XCOBTUNSZUJCDH-UHFFFAOYSA-B 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims description 50
- 150000001768 cations Chemical class 0.000 claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 239000011777 magnesium Substances 0.000 claims description 23
- 229910052744 lithium Inorganic materials 0.000 claims description 21
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 20
- 239000012530 fluid Substances 0.000 claims description 13
- KWLMIXQRALPRBC-UHFFFAOYSA-L hectorite Chemical compound [Li+].[OH-].[OH-].[Na+].[Mg+2].O1[Si]2([O-])O[Si]1([O-])O[Si]([O-])(O1)O[Si]1([O-])O2 KWLMIXQRALPRBC-UHFFFAOYSA-L 0.000 claims description 13
- 229910000271 hectorite Inorganic materials 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 13
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 7
- 125000003827 glycol group Chemical group 0.000 claims description 3
- 229920001451 polypropylene glycol Polymers 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims 1
- -1 polyethylene Polymers 0.000 claims 1
- 229920000573 polyethylene Polymers 0.000 claims 1
- 229920000151 polyglycol Polymers 0.000 claims 1
- 239000010695 polyglycol Substances 0.000 claims 1
- 239000011734 sodium Substances 0.000 abstract description 4
- 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 abstract description 3
- 229910052708 sodium Inorganic materials 0.000 abstract description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 abstract 1
- 150000002500 ions Chemical class 0.000 abstract 1
- 239000000047 product Substances 0.000 description 19
- 239000000391 magnesium silicate Substances 0.000 description 12
- 239000000499 gel Substances 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- FSBVERYRVPGNGG-UHFFFAOYSA-N dimagnesium dioxido-bis[[oxido(oxo)silyl]oxy]silane hydrate Chemical compound O.[Mg+2].[Mg+2].[O-][Si](=O)O[Si]([O-])([O-])O[Si]([O-])=O FSBVERYRVPGNGG-UHFFFAOYSA-N 0.000 description 9
- 235000019792 magnesium silicate Nutrition 0.000 description 9
- 229910052919 magnesium silicate Inorganic materials 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 239000002002 slurry Substances 0.000 description 8
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 7
- 239000013078 crystal Substances 0.000 description 7
- 239000006185 dispersion Substances 0.000 description 7
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 5
- 239000001095 magnesium carbonate Substances 0.000 description 5
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 5
- 239000002243 precursor Substances 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 229910019142 PO4 Inorganic materials 0.000 description 4
- 229940094522 laponite Drugs 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 235000021317 phosphate Nutrition 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000004927 clay Substances 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000010335 hydrothermal treatment Methods 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 235000012243 magnesium silicates Nutrition 0.000 description 3
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 3
- 235000019341 magnesium sulphate Nutrition 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 3
- 239000010452 phosphate Substances 0.000 description 3
- 238000000518 rheometry Methods 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- 229910001415 sodium ion Inorganic materials 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 2
- 241000871495 Heeria argentea Species 0.000 description 2
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 239000012736 aqueous medium Substances 0.000 description 2
- 239000007900 aqueous suspension Substances 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000002734 clay mineral Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 230000003111 delayed effect Effects 0.000 description 2
- 239000000645 desinfectant Substances 0.000 description 2
- 239000003599 detergent Substances 0.000 description 2
- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 description 2
- 238000005553 drilling Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 238000003898 horticulture Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000002453 shampoo Substances 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
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000008399 tap water Substances 0.000 description 2
- 235000020679 tap water Nutrition 0.000 description 2
- 230000009974 thixotropic effect Effects 0.000 description 2
- 239000000606 toothpaste Substances 0.000 description 2
- CEHZYZVJEXXYPM-NBOCEFNVSA-N (3s,8s,9s,10r,13s,14s,17r)-17-[(2s)-1-aminopropan-2-yl]-10,13-dimethyl-2,3,4,7,8,9,11,12,14,15,16,17-dodecahydro-1h-cyclopenta[a]phenanthren-3-ol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@@H](CN)C)[C@@]1(C)CC2 CEHZYZVJEXXYPM-NBOCEFNVSA-N 0.000 description 1
- 241000013355 Mycteroperca interstitialis Species 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 239000013011 aqueous formulation Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000001246 colloidal dispersion Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- IPGANOYOHAODGA-UHFFFAOYSA-N dilithium;dimagnesium;dioxido(oxo)silane Chemical compound [Li+].[Li+].[Mg+2].[Mg+2].[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O IPGANOYOHAODGA-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001595 flow curve Methods 0.000 description 1
- 230000000887 hydrating effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 150000002642 lithium compounds Chemical class 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 150000002892 organic cations Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 229910021647 smectite Inorganic materials 0.000 description 1
- 150000003388 sodium compounds Chemical class 0.000 description 1
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/40—Clays
- C01B33/405—Clays not containing aluminium
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The use of a non-hydrated synthetic magnesium silicate composition of the formula: [Si8(MgaLibHc)O20(OH)4-yFy]<z->. z/nM<n+> where a is 4.95 to 6.6, b is 0 to 1.5, c is 0 to <2, a+b+c is 5 to <8, Y IS 0 TO <4,Z =12-2A-B-C, M is a cation other than Li; to form a gelled aqueous composition. a gycol degelling agent may be added to the aqueous composition. The lithium-free forms of the silicate may have longer gelling times. The counter ion M may be Na (sodium).
Description
2401 1 03 Synthetic magnesium silicate compositions, methods and uses
thereof This invention is concerned with synthetic magnesium silicate compositions, methods and uses thereof. In particular, the present invention concerns the use of synthetic magnesium silicate compositions that contain reduced amounts of lithium or are lithium-free, lithium-free synthetic magnesium silicate compositions, methods of extending the gel time of aqueous compositions comprising synthetic magnesium silicate compositions and processes for the preparation of synthetic magnesium silicate compositions.
With the name "hectorite" has been ascribed to a natural trioctahedral smectite found at Hector, California, USA. This clay is an hydrous magnesium silicate having the ideal composition Sit Mg6 O20 (OH)4 modified by having a portion of the Mg+2 and OH- ions replaced by Li+ and F- ions.
The synthesis of hydrous magnesium silicates similar to natural hectorite has been described by Granquist and Pollack in "Clays and Clay minerals" Vol. 8 (Proceedings,.
of the 8 National Conference on Clays and Clay Minerals) pages 150-169. In the process described by Granquist, gels of magnesium hydroxide and of silica are produced separately, are washed, are combined and are redispersed in water to form a suspension. Lithium hydroxide or lithium fluoride and sodium hydroxide are added to.
the suspension that is then treated hydrothermally by refluxing it with stirring until a.
product having a crystal structure similar to that of hectorite is formed.
While Granquist's product has the crystal structure similar to natural hectorite it does not have good theological properties. Measuring the gingham Yield Value of an aqueous dispersion of the substance provides a standard yardstick of theological properties of a substance. The term gingham Yield Value (also known as gingham Yield Stress, these terms being alternatives for the same property) is referred to in standard works on rheology for example in "Rheology Theory and Applications" F R Eirich (Aced. Press) Vol. 1 (1956) page 658 and "Colloidal Dispersions" L K Fisher (N.Y. Bureau of Standards) 2nd Edition 1953, pages 150-170 and "The Chemistry and Physics of Clays and other Ceramic Materials" 3rd Edition, page463, A B Searle and R W Grimshaw.
The gingham Yield Value may be determined by first obtaining a flow curve relating the shear stress to the rate of shear and then extrapolating the straight line section of the curve to the shear stress axis, the intercept being the gingham Yield Value. It can conveniently be determined on any viscometer capable of measuring a range of shear rates and shear stresses.
The product of Granquist, when in the form of a dispersion obtained using 2g silicate and lOOml tap water, gives a gingham Yield Value of only about t5 dynes per cm2.
This is a very low value, inferior to that given by natural hectorite. It also gives a low static gel strength.
Processes for the production of synthetic hydrous magnesium silicate compositions having a crystal structure similar to natural hectorite but having better theological properties than natural hectorite have been described in GB-A-1054111, GB-A tol213122 and GB-A-1432770. À A Àe::: The process described in the GB-A-1054111 involves forming a slurry by co precipitation by slowly combining with heating and agitation in an aqueous medium a constituent providing the magnesium ions with constituents providing the silicon (as À. ..
silicates), hydroxyl and sodium ions and treating the precipitate hydrothermally to. . crystalline the synthetic mineral-like clay, washing and dewatering the resulting. . crystallized product, and drying the product at a temperature up to 450 C. The concentration of the slurry is desirably such that the concentration of the product formed is from 1% to 8% by weight, preferably 4% by weight. The hydrous synthetic magnesium silicate contains fluorine and lithium. The clay-like minerals provided have the structural formula: I (Sit Mg6 x Lix.020.(0H)4 y Fy)X() x/nMn( ) in which x is between O and 6, y is from 1 up to but excluding 4, and M is a cation, preferably Na+.
The process described in GB-A-1213122 involves precipitating a synthetic magnesium silicate by combining an aqueous solution of a water soluble magnesium salt with an aqueous alkaline solution of one or more sodium compounds *n the presence of dissolved silicon compound and hydrothermally treating the precipitate under pressure to crystallise the synthetic mineral-like clay, separating the resultant solid and liquid phases, washing the resulting crystallised product, and drying the product. The concentration of the precipitate is preferably not more than 5% by weight. The hydrous magnesium silicate product contains no fluorine, optionally contains lithium and has the general formula: [Si8MgaLibH4+co24]( 22abC) M( 2-2a-b-c)+ where (i) M is a sodium, a lithium or an equivalent of an organic cation, and (ii) the value of a, b, and c is such that either a<6, b>O, c>O, b+c<2, and (a+b+c-6)<2; or a<6, b=O, c,2 and (a+c-6)<2.
The process described in GB-A- 1432770 involves the synthesis of an hydrous magnesium silicate having a crystal structure similar to that of hectorite and having the general formula: [Sis (MgaLibHc)O2o(OH)4yFy]7r.zM+ wherein a is 4.95 to 5.7, b is from 0 to 1.05, c is from 0 to <2, a+b+c is from >4 to <8, y À ....
is from O to <4, z = 12-2a-b-c, and M is Na+ or Li+. The process comprises the..
sequential steps of forming an aqueous suspension of magnesium carbonate, forming a À.- silica precipitate in the aqueous suspension magnesium carbonate, the proportions of À ., . magnesium provided by the magnesium carbonate and silica precipitated in the À ..
suspension corresponding to that of the formula of the magnesium silicate, maintaining. . the resulting mixture of magnesium carbonate and silica in the wet state and subjecting. À . it to hydrothermal treatment by heating it in an aqueous medium and in the presence of the remaining constituents of the magnesium silicate in proportions within the ranges specified in the general formula and in the presence of excess dissolved sodium or lithium compound over that required to form the cation ofthe magnesium silicate until crystal growth occurs and separating the resulting crystalline product. The crystalline material resulting from the hydrothermal treatment is then separated by filtration, washed, and dried at a temperature not exceeding 450 C. The process described in GB A1432770 is distinguished from the processes described in GB-A-1054111 and GB-A 1213122 in that, in those processes, the Mg compound and the silica are co-precipitated.
Though GB-A-1432770 discloses a general formulation for a synthetic magnesium silicate composition in which there is a possibility for the composition to be lithium free, there is no explicit disclosure in GB-A1432770, or in any other prior art, which indicates a lithium-free composition ever having been prepared.
The processes described in GB-A-1432770, GB-A-1054111 and GB-A-1213122 are generally batch processes. Continuous processes for the preparation of synthetic magnesium silicates are described in Japanese Patent Application No 06-345419 and in UK Patent Application No 0229630.9, filed 20'h December 2002.
The products of the processes described in the above prior art documents are characterized by providing dispersions having gingham Yield Values substantially in excess of any known to be given by natural hectorite dispersions. Some of these products have found widespread use, by virtue of their excellent theological properties, in many applications, including in paints and other surface coatings; cosmetic products; horticulture; shampoos; detergents; disinfectants; toothpastes; paper manufacture, for example as fillers, retention and drainage aids, and in paper coatings; and drilling muds. . ....
The products of the above batch processes are commercially available as dry white. À powders, such as the products sold by Rockwood Additives Limited, England, under the trademark "LAPONITE" and, when fully dispersed and hydrated in water, the resulting composition is colourless and transparent. À ..
As mentioned above, synthetic magnesium silicate compositions are characterized by.. . providing dispersions having gingham Yield Values substantially in excess of any known natural hectorite dispersions, and have resulted in their use, by virtue of their excellent theological properties, in various applications including in surface coatings.
The free flowing white powder takes no more than an hour at ambient temperatures from it being dispersed under shear in water at a level from 1% by wt to hydrate sufficiently to form a highly viscous, thixotropic gel. The time required to form the gel can be reduced by using increased temperatures and by using higher shearing conditions.
It is known, for example from an inspection of the www.laponite.com website, that at concentrations of above 2% by wt synthetic magnesium silicate in tap water, highly thixotropic gels are formed(substantially less than one hour e.g a 5% by wt aqueous composition may gel in 5 minutes), which can make it difficult to incorporate other raw materials into the formulation. Accordingly, if the concentration of synthetic magnesium silicate to be used is above 2% by wt. the use of a degelling agent, such as tetrasodium pyrophosphate or a low molecular weight polyethylene glycol, is often recommended.
Whilst the onset of gelling can be delayed by the presence of a degelling agent, some applications of the end formulation, such as coatings for some metals, do not permit the presence of condensed phosphates. Further, it may be more convenient in a manufacturing process not to have to rely upon the presence of a degelling agent.
It is an object of the present invention to delay the onset of gelling in aqueous formulations comprising synthetic magnesium silicate compositions. It is another object to provide synthetic magnesium silicate compositions which demonstrate delayed gelling properties. It is another object of the present invention to reduce or eliminate the amount of degelling agent e.g. phosphate used in an aqueous synthetic magnesium. ..
silicate compositions. Preferably, the delay in gelling will occur without having any..
detrimental effects on the final properties of the gelled composition. À: :e
In accordance with a first aspect of the present invention, there is provided the use of a À non-hydrated synthetic magnesium silicate compostion of Formula I below: .. *, I.- À ..', Formula l [Sia (MgaLibHc)020(0H)4 yFy]Z- %Mn+ whereinais4.95to6.6,bis from Oto 1.5, cishromOto<2,a+b+cistromSto<8,yis from O to <4, z = 12-2a-c, M is a cation which is other than Li, and n is the valency of M, wherein the ratio of Si:Mg is from 8:6.6 to 8:4.95 in a method for the preparation of an aqueous composition comprising said synthetic magnesium silicate composition in a hydrated form, which method comprises adding under mLxing conditions said non-hydrated synthetic magnesium silicate composition to an aqueous fluid and allowing said non-hydrated synthetic magnesium silicate composition to hydrate.
In another aspect, the present invention provides the use of a nonhydrated synthetic magnesium silicate composition of Formula I below: Formula I [Sis (MgaLibH')020(0H)4yFy]Z.7/nM wherein a is 4.95 to 6.6, b is from O to 1.5, c is from O to <2, a+b+c is from 5 to <8, y is from O to <4, z = 12-2a-c, M is a cation which is other than Li, and n is the valency of M, wherein the ratio of Si:Mg is from 8:6.6 to 8:4.95in a method for the preparation of a gelled aqueous composition comprising said synthetic magnesium silicate composition in a hydrated form, which method comprises adding under mixing conditions said non l O hydrated synthetic magnesium silicate composition to an aqueous fluid and allowing said non-hydrated synthetic magnesium silicate composition to hydrate, for delaying gelling of said gelled aqueous composition.
In another aspect, the present invention provides a method of reducing or eliminating the amount of degelling agent used in the preparation of an aqueous composition comprising a synthetic magnesium silicate composition in hydrated form, which method if comprises adding under mixing conditions a non-hydrated synthetic magnesium silicate..
composition of Formula 1: Formula I..
[Sit (MgaLibHC)o2o(oH)4-yFy]Z-.Z/nMn À.
wherein a is 4.95 to 6.6, b is from O to 1.5, c is from O to <2, a+b+c is from 5 to <8, y is, . from O to <4, z = 12-2a-b-c, M is a cation which is other than Li, and n is the valency of M, wherein the ratio of Si:Mg is from 8:6.6 to 8:4.95 to an aqueous fluid and allowing said non-hydrated synthetic magnesium silicate composition to hydrate.
In another aspect, there is provided an aqueous composition comprising an aqueous fluid and a synthetic magnesium silicate composition of Formula l: Formula I [Sit (MgaLibHc)020(0H)4yFy]Z.z/nMn wherein a is 4.95 to 6.6, b is from O to 1.5, c is from O to <2, a+b+c is from 5 to <8, y is from O to <4, z = 1 2-2a-b-c, M is a cation which is other than Li and n is the valency of M, wherein the ratio of Si:Mg is from 8:6.6 to 8:4.95 Preferably, the synthetic magnesium silicate composition used in the preset invention is completely free of Li. Such a composition preferably has the composition of Formula II below: Formula II [Six (MgHc)02o(0H)4 yFy]7.7/nMn+ whereinais4.95to6.6,cisfromOto<2,a+ eisbrom5to<8,yisbromOto<4,z= 12 2a-c, M is a cation which is other than Li, and n is the valancy of M, wherein the ratio of Si:Mg is from 8:6.6 to 8:4.95 In accordance with another aspect ofthe present invention there is provided a synthetic magnesium silicate composition of Formula II below: Formula 11 [Six (MgaHc)o2o(oH)4yFyz-%Mn+ wherein a is 4.95 to 6.6, c is from O to <2, a+c is from 5 to <8, y is from O to <4, z= 12 2a-c, M is a cation which is other than Li, and n is the valancy of M, wherein the ratio of Si:Mg is from 8:6.6 to 8:4.95 In the synthetic magnesium silicate compositions of Formula I and Formula 2: a) the Si:Mg ratio is prefereably from 8:5.8 to 8:5.3, more preferably from 8:5.68 to 8:5.42; b) the M+ cation is preferably Ma+, c) y is preferably from O to 3.
It has been found that by reducing or eliminating the amount of Li in the synthetic magnesium silicate composition and employing a specific Si:Mg ratio, the time within which the composition gels once it has been added to water or other aqueous fluid is extended. For example, it can be demonstrated that an aqueous composition formed by the addition to water under conventional mixing conditions at room temperature of a synthetic magnesium silicate composition of Formula II in an amount of 5 wt % may take well over an hour before it forms a highly viscous, gelled composition. Further, once the composition has gelled, its theological properties are substantially similar to the aqueous gels formed from hydrating conventional highcontent lithium magnesium silicate compositions. This finding is very surprising and, at present, cannot be explained by the inventors.
The ability to delay gelling without loss of final gel properties offers significant advantages over the conventional compositions. For example, it enables the preparation of aqueous compositions comprising higher amounts of synthetic magnesium silicate compositions than would normally be possible with conventional lithium containing magnesium silicates. Further, aqueous compositions can be prepared which contain reduced or no degelling agents e.g. phosphate free coatings may now be available for use in the metal finishing industry.
The compositions of Formula I may be prepared by the processes detailed in GB-A 1054111, GB-A-tol213122, GB-A-1432770, Japanese Patent Application No 06 345419 and UK Patent Application No 0229630.9, which are incorporated herein by reference. 1 The compositions of Formula II may be prepared by a similar procedure as detailed in GB-A-1054111, GB-A-tol213122, GB-A1432770, Japanese Patent Application No 06-345419 and UK Patent Application No 0229630.9, except that all Li- containing.
compounds are absent. Accordingly, in another aspect, the present invention provides a..
method of preparing a synthetic magnesium silicate composition of Formula II, having a À À crystal structure similar to natural hectorite, wherein the process comprises the steps of...
a) forming a precursor slurry by mixing and reacting together water, magnesium À sulphate, sodium carbonate and sodium silicate, b) subjecting said precursor slurry to a hydrothermal reaction at a temperature offrom 210 to 400 C, and c) washing and À À À À filtering to remove water soluble salts formed in the preparation of the precursor slurry. À . . .: 25; The composition of Formula II retains substantially similar theological properties to the products formed in GB-A-1054111, GB-A- 1213122 and GB-A-1432770. The compositions may be supplied as dry white powders or as moist solids or in dispersions.
Accordingly, the compositions may be used in the same type of applications as the prior art products. For example, the compositions may be used in paints; cosmetic products; horticulture; shampoos; detergents; disinfectants, toothpastes; paper manufacture, for example as fillers, retention and drainage aids, and in paper coatings; and drilling muds.
The Li-free compositions of Formula II, may additionally be useful in applications in which the product is intended to be consumed, such as in food and medicinal applications.
In yet another aspect, the present invention provides a method of extending the gelling time of an aqueous composition comprising a synthetic magnesium silicate composition in hydrated form and a degelling agent, such as a glycol or a phosphate, which method comprises adding under mixing conditions a non-hydrated synthetic magnesium silicate having a structure similar to natural hectorite, preferably as made by any of the processes claimed in GB-A-1432770, GB-A-1054111, GB-A-1213122, Japanese Patent Application No 06-345419 and in UK Patent Application No 0229630.9 (filed 20th December 2002), to an aqueous fluid and allowing said non-hydrated synthetic magnesium silicate composition to hydrate, characterized in that the aqueous fluid into which said non-hydrated composition is added comprises at least 80% by weight, preferably 100 % by weight, of the degelling agent used in the aqueous composition. In one particular embodiment, the degelling agent is a glycol, which is preferably selected from one or more of ethylene glycol, propylene glycol, polyethylene glycol and polypropylene glycol. Preferably, the nonhydrated synthetic magnesium silicate.
composition is of Formula I: . Formula I [Sit (MgaLibH:)020(0H)4 yFy]Z-.Z/nM À . wherein a is 4.95 to 6.6, b is from O to l.5, c is from O to <2, a+b+c is from S to <8, y is: . À.
from O to <4, z = 12-2a-b-c, M is a cation which is other than Li, and n is the valency of M, wherein the ratio of Si:Mg is from 8:6.6 to X:4.95. More preferably, the synthetic À À À magnesium silicate composition is of Formula II below: À . . .: Formula II [Sig (MgaHc)o2o(oH)4-yFy]z- %Mn+ whereinais4.95to6.6,cisbromOto<2,a+ cisfromSto<8,yistromOto<4,z= 12 2a-c, M is a cation which is other than Li, and n is the valancy of M, wherein the ratio of Si:Mg is from 8:6.6 to 8:4.95.
The following examples illustrate aspects of the invention, but are not in any way intended to limit the scope the invention.
Various synthetic magnesium silicate compositions were prepared by the procedure detailed in Examples 1 and 2 below from the amounts of raw materials, as indicated in
Table 1:
Example 1 - Preparation of precursor slurry (bulk preparation) A measured quantity of magnesium sulphate and water (sufficient to dissolve the measured quantity of magnesium carbonate) is placed in a flask fitted with a stirrer, a heating mantle and a refluxing condenser. The mixture was brought to a temperature of at least 60 C under reflux while stirring efficiently.
From a separate vessel a measured quantity of sodium carbonate solution is added slowly to the reaction vessel containing the magnesium sulphate solution. The addition is made over a period of up to one hour, while the reaction mixture is kept at 60 C or greater and stirred efficiently throughout.
From a separate vessel a measured quantity of sodium silicate solution is added slowly to the reaction vessel containing the magnesium sulphate and sodium carbonate.
solution. The addition is made over a period of up to one hour, while the reaction.
mixture is kept at 60 C or greater and stirred efficiently throughout. À..
The mixture is then boiled under reflux, with efficient stirring, for about 2 hours. À Example 2 - Hydrothermal treatment (bulk preparation) The precursor slurry obtained in each of Example 1 was fed into a reactor having an internal temperature of 200 C and pressure of 16 barg. The slurry now undergoes a hydrothermal reaction. The material is retained in the reactor for up to 18 hours, before it is ejected from the reactor into a bath where magnesium silicate crystal so formed are wash and filtered to remove soluble salts.
After being drying at 1 05 C and milled to particle size of no greater than 250 microns, the rheology properties of the powders so produced were evaluated. The results of the evaluation are also presented in Table 1.
From Table 1, it is evident that compositions comprising reduced or no lithium develop gelling properties more slowly than the conventional composition Laponite RD.
Laponite RD is a synthetic magnesium silicate of the typical formula [Sis(Mgs sLio 3Ho 2)020(0H)4] 5 o sNa+, available from Rockwood Additives Limited, England.
Viscosity was measured at 25 C using a number 4 Ford viscosity cup. The unit of measurement for this method is 'seconds'. À À À À. À À . À À. À:. :. À... À.. À À À .
- -
3 _ u, _ _ a _ a _ iS
_ _ _ _ _ _ _ _ _ _ _ _ L _ _
O _ O _ O _ O _ O _ O _ O _ N O
a. , ' : :.
_ _ _ -- _ _ _ _:: _ X. _ 0,0 _ _ _ vm0 _ iO,, _ o.0 O,, _ _ _ __s -i-( :...
_ C_ _ _ _c _ = _ C S = cn V q eq & w 5' _ _ n n- v- g l? 1: MEL e r. _ A _ _ _ _ D V _ W. 5= v _ -- _ 2 Q 2 _ _ of...
o X it, _ e 3 _ _ _ Y À.-..
e c _ ___ n! BE: BE an 1' S r LL L Ll
Claims (16)
- - Is - Claims 1. The use of a non-hydrated synthetic magnesium silicatecomposition of Formula I below: Formula I [Six (MgaLibHc)o2o(oH)4-yFyz-%Mn+ wherein a is 4.95 to 6.6, b is from O to 1.5, c is from O to <2, ab+c is from 5 to <8, y is from O to <4, z = 12-2a-b-c, M is a cation which is other than Li, and n is the valency of M, wherein the ratio of Si:Mg is from 8:6.6 to 8:4.95 in a method for the preparation of an aqueous composition comprising said synthetic magnesium silicate composition in a hydrated form, which method comprises adding under mixing conditions said non-hydrated synthetic magnesium silicate composition to an aqueous fluid and allowing said non-hydrated synthetic magnesium silicate composition to hydrate.
- 2. The use of a non-hydrated synthetic magnesium silicate composition of Formula.I below: . Formula I [Sit (MgaLibHc)020(0H)4yFy]Z Z/nMn À À wherein a is 4.95 to 6.6, b is from O to 1.5, c is from O to <2, a+b+c is from 5 to <8, y is.. . from O to <4, z = 12-2a-b-c, M is a cation which is other than Li, and n is the valency of M, wherein the ratio of Si:Mg is from 8:6.6 to 8:4.95 À À in a method for the preparation of a gelled aqueous composition comprising said À À À synthetic magnesium silicate composition in a hydrated form, which method comprises adding under mixing conditions said non-hydrated synthetic magnesium silicate composition to an aqueous fluid and allowing said non-hydrated synthetic magnesium silicate composition to hydrate, for delaying gelling of said gelled aqueous composition.
- 3. A method of reducing or eliminating the amount of degelling agent used in the preparation of an aqueous composition comprising a synthetic magnesium silicate composition in hydrated form, which method comprises adding under mixing conditions a non-hydrated synthetic magnesium silicate composition of Formula I: Formula I [Sib (MgaLibHc)o2o(oH)4-yFy]z-.%Mn+ whereinais4.95to6.6,bistromOto 1.5, cisfromOto<2,a+b+cistrom5to<8,yis Dom O to <4, z = 12-2a-b-c, M is a cation which is other than Li, and n is the valency of M, wherein the ratio of Si:Mg is from 8:6.6 to 8:4.95 to an aqueous fluid and allowing said non-hydrated synthetic magnesium silicate composition to hydrate.
- 4. An aqueous composition comprising an aqueous fluid and a synthetic magnesium silicate composition of Formula 1: Formula I [Sit (MgaLibHc)020(0H)4 yFy] .%M wherein a is 4.95 to 6.6, b is from O to 1.5, c is from O to <2, a+b+c is from S to <8, y is from O to <4, z = 122a-b-c, M is a cation which is other than Li, and n is the valency of M, wherein the ratio of Si:Mg is from 8:6.6 to 8:4.95
- 5. The use of claim 1 or claim 2, method of claim 3 or composition of claim 4, wherein the synthetic magnesium silicate composition is free of Li. ....
- 6. The use of claim 1 or claim 2, method of claim 3 or composition of claim 4, À À wherein the non-hydrated synthetic magnesium silicate composition is of Formula II.. . below: ....Formula II À [Six (MgaHc)o2o(oH)4yFy] . /nM À. À: wherein a is 4.95 to 6.6, c is from O to <2, a+c is from 5 to <8, y is from O to <4, z = 12 2a-c, M is a cation which is other than Li, and n is the valancy of M, wherein the ratio of Si:Mg is from 8:6.6 to 8:4.95.
- 7. The use, method, or composition as claimed in any one of the preceding claims, wherein the aqueous composition comprises a degelling agent. I
- 8. The use, method or composition of claim 7, wherein the degelling agent is a glycol, preferably ethylene glycol, propylene glycol or a low molecular weight polyglycol.
- 9. A synthetic magnesium silicate composition of Formula II below: Formula II [Sis (MgaNc)020(0H)4 yFy]Z-.zlnMn+ wherein a is 4.95 to 6.6, c is from O to <2, a+c is from S to <8, y is from O to <4, z = 12 2a-c, M is a cation which is other than Lit and n is the valancy of M, wherein the ratio of Si:Mg is from 8:6.6 to 8:4.95
- 10. A method of extending the gelling time of an aqueous composition comprising a synthetic magnesium silicate composition in hydrated form and degelling agent, preferably a glycol, which method comprises adding under mixing conditions a non hydrated synthetic magnesium silicate having a structure similar to natural hectorite, preferably as made by any ofthe processes claimed in GB-A-1432770, GB-A-1054111, GB-A-1213122, Japanese Patent Application No 06-345419 and in UK Patent Application No 0229630.9 (filed 20'h December 2002), to an aqueous fluid and allowing said non-hydrated synthetic magnesium silicate composition to hydrate, characterized in that the aqueous fluid into which said non-hydrated composition is added comprises at. . least 80% by weight, preferably 100 % by weight, of the degelling agent used in the.aqueous composition.
- 11. The method of claim 1 O. wherein the degelling agent is a glycol, preferably a., À glycol selected from one or more of ethylene glycol, propylene glycol, polyethylene....glycol and polypropylene glycol. . . eel-
- 12. The method of claim 11 or claim 12, wherein the non-hydrated synthetic magnesium silicate composition is of Formula I: Formula I [sib (MgaLibHC)o2o(oH)4-yFy]Z- zlnMn wherein a is 4.95 to 6.6, b is from O to 1.5, c is from O to <2, a+b+c is from 5 to <8, y is from O to <4, z = 12-2a-b-c, M is a cation which is other than Lit and n is the valency of M, wherein the ratio of Si:Mg is from 8:6.6 to 8:4.95.
- 13. The method of claim 12, wherein the synthetic magnesium silicate composition is of Formula II below: Formula II LSis (Mg8)O20(0H)4 yFy]z%M wherein a is 4.95 to 6.6, c is from 0 to <2, a+c is from 5 to <8, y is from 0 to <4, z = 12 2a-c, M is a cation which is other than Li, and n is the valancy of M, wherein the ratio of Si:Mg is from 8:6.6 to 8:4.95.
- 14. The use, method, or composition as claimed in any one ofthe preceding claims, wherein the Si:Mg ratio in the synthetic magnesium silicate composition is from 8:5.8 to 8:5.3, preferably from 8:5.68 to 8:5.42.
- 15. The use, method, or composition as claimed in any one of the preceding claims, wherein the Mt cation in the synthetic magnesium silicate composition is Ma+
- 16. The use, method, or composition as claimed in any one of the preceding claims, wherein y in the synthetic magnesium silicate composition is from 0 to 3. À. Àe a me a :'e. . . Àe À- Àe e.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB0309620A GB2401103A (en) | 2003-04-29 | 2003-04-29 | Synthetic magnesium silicate compositions, methods and uses |
| PCT/GB2004/001767 WO2004096708A1 (en) | 2003-04-29 | 2004-04-23 | Synthetic magnesium silicate compositions, methods and uses thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| GB0309620A GB2401103A (en) | 2003-04-29 | 2003-04-29 | Synthetic magnesium silicate compositions, methods and uses |
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| US8895476B2 (en) | 2011-03-08 | 2014-11-25 | Tetra Technologies, Inc. | Thermal insulating fluids |
| CN104760966B (en) * | 2015-03-27 | 2017-06-13 | 中国地质大学（武汉） | A kind of method of Mechano-chemical Synthesizing lithium magnesium silicate |
| DE102024121958A1 (en) | 2023-08-11 | 2025-02-13 | Devinochem GmbH & Co.KG | Layered silicate, process for its preparation and its use |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1213122A (en) * | 1966-09-12 | 1970-11-18 | Laporte Industries Ltd | Clays |
| GB1294253A (en) * | 1971-01-04 | 1972-10-25 | Pfizer | Use of synthetic clay containing no lithium as soil anti-redeposition agent, in detergents |
| GB1376379A (en) * | 1971-05-24 | 1974-12-04 | Pfizer | Use of synthetic clays containing fluorine and lithium as soil anti-redeposition agents in detergents |
| GB1432770A (en) * | 1972-11-14 | 1976-04-22 | Laporte Industries Ltd | Production of magnesium silicates |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1276016A (en) * | 1969-06-10 | 1972-06-01 | Laporte Industries Ltd | Synthetic silicate compositions |
| JPS5320959B2 (en) * | 1973-05-14 | 1978-06-29 | ||
| US4054537A (en) * | 1976-04-26 | 1977-10-18 | N L Industries, Inc. | Process for synthesizing compositions containing smectite-type clays and gellants produced thereby |
| DE3526405A1 (en) * | 1985-07-24 | 1987-02-05 | Henkel Kgaa | LAYERED SILICATES WITH RESTRICTED SOURCE, PROCESS FOR THEIR PRODUCTION AND THEIR USE IN DETERGENT AND CLEANING AGENTS |
| GB9301456D0 (en) * | 1993-01-26 | 1993-03-17 | Laporte Industries Ltd | Synthetic clay minerals |
-
2003
- 2003-04-29 GB GB0309620A patent/GB2401103A/en not_active Withdrawn
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2004
- 2004-04-23 WO PCT/GB2004/001767 patent/WO2004096708A1/en active Application Filing
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1213122A (en) * | 1966-09-12 | 1970-11-18 | Laporte Industries Ltd | Clays |
| GB1294253A (en) * | 1971-01-04 | 1972-10-25 | Pfizer | Use of synthetic clay containing no lithium as soil anti-redeposition agent, in detergents |
| GB1376379A (en) * | 1971-05-24 | 1974-12-04 | Pfizer | Use of synthetic clays containing fluorine and lithium as soil anti-redeposition agents in detergents |
| GB1432770A (en) * | 1972-11-14 | 1976-04-22 | Laporte Industries Ltd | Production of magnesium silicates |
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