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US4049780A Expired / Lapsed US ⏱️ 0.0 years remaining

Production of magnesium silicates

Assignee: Evonik LIL Ltd
•
Filing: 1976-05-18
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Granted: 1977-09-20
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Expires: 1996-05-18
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Abstract

Abstract Hydrous magnesium silicates having a crystal structure similar to that of natural hectorite may be produced by a precipitation process in which silica is precipitated into a preformed aqueous suspension of a water insoluble magnesium compound. The process may be operated at high concentration and the products may have good dispersibility in aqueous media and high optical clarity when dispersed as well as the good rheological properties which may be obtained by prior precipitation processes.

Inventors

  • 👤 Barbara Susan Neumann

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-24 13:03
CPC Classifications
C; C01; C01B; C01B33/00; C01B33/20; C01B33/36; C01B33/38; C01B33/40; C01B33/405

Claims Analysis

Total Claims: 12
Claim 1
Independent Claim 373 words
A process for the synthesis of a hydrous magnesium silicate having an X-ray diffraction pattern indicative of a hectorite structure and having a Bingham Yield Value of from 40 to 250 dynes/cm 2 and having the general formula [Si.sub.8 (Mg.sub.a Li.sub.b H.sub.c)O.sub.20 (OH).sub.4-y F.sub.y ] .sup.z- ZM.sup.+ wherein a, b, c, y, z and M have the values: 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 is from 0 to 4 z = 12-2a-b-c M is Na+ or Li+ comprising the steps of: a. forming an aqueous suspension of magnesium carbonate by dissolving a suitable water soluble magnesium compound in water, precipitating magnesium carbonate by adding to the resulting solution an aqueous solution of sodium carbonate; b. adding to a suspension of the freshly precipitated magnesium carbonate a water soluble silicon compound; c. precipitating silica into the suspension of freshly precipitated magnesium carbonate by reacting the water soluble silicon compound with sodium carbonate; the total time for addition in step (a) and in step (b) being at least 30 minutes, d. adding during or after step (a) or (b) or (c) lithium or fluorine ions if required by the general formula above; e. controlling the quantity of magnesium carbonate and silicon precipitated and the quantity of lithium or fluorine ions added to give a Si:Mg:Li:F ratio within the ranges stated in the general formula above; f. controlling the concentrations of the reactants used in steps (a), (b) and (e) to give a suspension having a concentration of solids at least 5% by weight; g. maintaining the solids in the wet state; h. treating the wet solids as a suspension having a concentration of at least 5% by weight in water in the presence of an excess of sodium or lithium ions of from 25 to 250% over that providing the cation M in the general formula above by heating it to cause crystal growth of the hydrous magnesium silicate of the above formula for from 1 to 20 hours at a pressure at least equal to atmospheric pressure while maintaining the presence of water in the liquid state; and i. separating the resulting crystalline hydrous magnesium silicate.
Claim 2
Dependent Claim 373 words
A process for the synthesis of a hydrous magnesium silicate having an X-ray diffraction pattern indicative of a hectorite structure and having a Bingham Yield Value of from 40 to 250 dynes/cm 2 and having the general formula [Si.sub.8 (Mg.sub.a Li.sub.b H.sub.c)O.sub.20 (OH).sub.4-y F.sub.y ] .sup.z- ZM.sup.+ wherein a, b, c, y, z and M have the values: 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 is from 0 to 4 z = 12-2a-b-c M is Na+ or Li+ comprising the steps of: a. forming an aqueous suspension of magnesium carbonate by dissolving a suitable water soluble magnesium compound in water, precipitating magnesium carbonate by adding to the resulting solution an aqueous solution of sodium carbonate; b. adding to a suspension of the freshly precipitated magnesium carbonate a water soluble silicon compound; c. precipitating silica into the suspension of freshly precipitated magnesium carbonate by reacting the water soluble silicon compound with sodium carbonate; the total time for addition in step (a) and in step (b) being at least 30 minutes, d. adding during or after step (a) or (b) or (c) lithium or fluorine ions if required by the general formula above; e. controlling the quantity of magnesium carbonate and silicon precipitated and the quantity of lithium or fluorine ions added to give a Si:Mg:Li:F ratio within the ranges stated in the general formula above; f. controlling the concentrations of the reactants used in steps (a), (b) and (e) to give a suspension having a concentration of solids at least 5% by weight; g. maintaining the solids in the wet state; h. treating the wet solids as a suspension having a concentration of at least 5% by weight in water in the presence of an excess of sodium or lithium ions of from 25 to 250% over that providing the cation M in the general formula above by heating it to cause crystal growth of the hydrous magnesium silicate of the above formula for from 1 to 20 hours at a pressure at least equal to atmospheric pressure while maintaining the presence of water in the liquid state; and i. separating the resulting crystalline hydrous magnesium silicate.
Claim 3
Dependent Claim 27 words
A process as claimed in claim 1 wherein the total time of addition in step (a) and in step (b) is from 30 minutes to 4 hours.
Claim 4
Dependent Claim 390 words
A process for the synthesis of a hydrous magnesium silicate having an X-ray diffraction pattern indicative of a hectorite structure having a Bingham Yield Value of from 40 to 250 dynes/cm 2 and having the general formula [Si.sub.8 (Mg.sub.a Li.sub.b H.sub.c)O.sub.20 (OH).sub.4-y F.sub.y ] .sup.z- ZM.sup.+ wherein a, b, c, y, z and M have the values: 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 is from 0 to <4 z = 12-2a-b-c M is Na + or Li + comprising the steps of: a. forming an aqueous suspension of magnesium carbonate by dissolving a suitable water soluble magnesium compound in water, precipitating magnesium carbonate by adding to the resulting solution sodium carbonate, said precipitation being conducted over a period of time of from 30 minutes to 3 hours, and suspending the freshly precipitated magnesium carbonate; b. adding to the freshly precipitated magnesium carbonate a water soluble silicon compound; c. precipitating silica into the suspension of freshly precipitated magnesium carbonate by reacting the water soluble silicon compound with sodium carbonate, the precipitation of silica being conducted over a period of time from 15 minutes to 1 hour; d. adding during or after step (a) or (b) or (c) lithium or fluorine ions if required by the general formula above; (e) controlling the quantity of magnesium carbonate and silica precipitated and the quantity of lithium or fluorine ions added to give a Si:Mg:Li:F ratio within the ranges stated in the general formula above; f. controlling the concentrations of the reactants used in steps (a), (b) and (e) to give a suspension having a concentration of solids at least 5% by weight; g. maintaining the solids in the wet state; h. treating the wet solids as a suspension having a concentration of at least 5% by weight in water in the presence of an excess of sodium or lithium ions of from 25 to 250% over that providing the cation M in the general formula above by heating it to cause crystal growth of the hydrous magnesium silicate of the above formula for from 1 to 20 hours at a pressure at least equal to atmospheric pressure while maintaining the presence of water in the liquid state; and i. separating the resulting crystalline hydrous magnesium silicate.
Claim 5
Dependent Claim 390 words
A process for the synthesis of a hydrous magnesium silicate having an X-ray diffraction pattern indicative of a hectorite structure having a Bingham Yield Value of from 40 to 250 dynes/cm 2 and having the general formula [Si.sub.8 (Mg.sub.a Li.sub.b H.sub.c)O.sub.20 (OH).sub.4-y F.sub.y ] .sup.z- ZM.sup.+ wherein a, b, c, y, z and M have the values: 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 is from 0 to <4 z = 12-2a-b-c M is Na + or Li + comprising the steps of: a. forming an aqueous suspension of magnesium carbonate by dissolving a suitable water soluble magnesium compound in water, precipitating magnesium carbonate by adding to the resulting solution sodium carbonate, said precipitation being conducted over a period of time of from 30 minutes to 3 hours, and suspending the freshly precipitated magnesium carbonate; b. adding to the freshly precipitated magnesium carbonate a water soluble silicon compound; c. precipitating silica into the suspension of freshly precipitated magnesium carbonate by reacting the water soluble silicon compound with sodium carbonate, the precipitation of silica being conducted over a period of time from 15 minutes to 1 hour; d. adding during or after step (a) or (b) or (c) lithium or fluorine ions if required by the general formula above; (e) controlling the quantity of magnesium carbonate and silica precipitated and the quantity of lithium or fluorine ions added to give a Si:Mg:Li:F ratio within the ranges stated in the general formula above; f. controlling the concentrations of the reactants used in steps (a), (b) and (e) to give a suspension having a concentration of solids at least 5% by weight; g. maintaining the solids in the wet state; h. treating the wet solids as a suspension having a concentration of at least 5% by weight in water in the presence of an excess of sodium or lithium ions of from 25 to 250% over that providing the cation M in the general formula above by heating it to cause crystal growth of the hydrous magnesium silicate of the above formula for from 1 to 20 hours at a pressure at least equal to atmospheric pressure while maintaining the presence of water in the liquid state; and i. separating the resulting crystalline hydrous magnesium silicate.
Claim 6
Dependent Claim 35 words
A process as claimed in claim 1 wherein the precipitation of the water insoluble magnesium compound and of the silica is performed under conditions of stirring at a speed of below 200 revolutions per minute.
Claim 7
Dependent Claim 51 words
A process as claim in claim 1 wherein the concentrations of the reactants used in steps (a), (b) and (d) are controlled to give a suspension having a concentration of solids of at least 7% by weight and wherein the value of (b) in the general formula is up to 0.5.
Claim 8
Dependent Claim 21 words
A process as claimed in claim 5 wherein the suspension has a concentration of up to 10% of solids by weight.
Claim 9
Dependent Claim 11 words
A process as claimed in claim 1 wherein M is sodium.
Claim 10
Dependent Claim 30 words
A process as claimed in claim 1 wherein the suspension having a concentration of at least 5% produced by steps (a) to (f) is directly treated according to step (h).
Claim 11
Dependent Claim 23 words
A process as claimed in claim 1 wherein the suspension produced by steps (a) to (f) is boiled to expel CO 2 .
Claim 12
Dependent Claim 65 words
A process as claimed in claim 9 wherein the concentrations of the reactants used in steps (a), (b) and (d) are controlled to give a suspension having a concentration of at least 7% by weight wherein the value of (b) in the general formula is up to 0.5, and wherein the suspension produced by steps (a) to (f) is directly treated according to step (h).

References Cited (Backward Citations)

CA666992A Cited
US1999210A Cited
GB602453A Cited
GB1054111A Cited
GB1155595A Cited
US3586478A Cited
GB1121501A Cited
GB1213122A Cited
US3671190A Cited
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US3954943A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1980-09-19 1981-03-21 1981-09-20 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1984-09-19 1985-03-21 1985-09-20 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1988-09-19 1989-03-21 1989-09-20 $7700.00 Window Closed / Lapsed

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