US4717773A — Silicate esters and organosilicon compounds

Claim 1

Independent Claim 43 words

A method for preparing alkoxysilanes and alkoxysiloxanes which comprises treating a metal silicate with a solution of anhydrous or aqueous acid in an alcohol, heating the resulting mixture and removing low boiling components from said mixture, then isolating the product from the residue.

Claim 2

Independent Claim 43 words

A method for preparing alkoxysilanes and alkoxysiloxanes which comprises treating a metal silicate with a solution of anhydrous or aqueous acid in an alcohol, heating the resulting mixture and removing low boiling components from said mixture, then isolating the product from the residue.

Claim 3

Dependent Claim 15 words

The method of claim 1 wherein the silicate is a metal salt of silicon dioxide.

Claim 4

Dependent Claim 15 words

The method of claim 1 wherein the silicate is a salt containing the orthosilicate ion.

Claim 5

Dependent Claim 41 words

The method of claim 3 wherein the silicate is selected from the group consisting of beta-Ca 2 SiO 4 , gamma-Ca 2 SiO 4 , Ca 3 SiO 5 , CaMgSiO 4 and Zn 2 SiO 4 , or mixtures thereof.

Claim 6

Dependent Claim 13 words

The method of claim 1 wherein the silicate is a linear oligomeric silicate.

Claim 7

Dependent Claim 43 words

The method of claim 5 wherein the silicate is selected from the group consisting of Zn 4 Si 2 O 7 (OH) 2 .2H 2 O, Ca 2 MgSi 2 O 7 and Ca 3 Si 2 O 7 , or mixtures thereof.

Claim 8

Dependent Claim 13 words

The method of claim 1 wherein the silicate is a linear polymeric silicate.

Claim 9

Dependent Claim 23 words

The method of claim 7 wherein the silicate is selected from the group consisting of CaSiO 3 , BaSiO 3 or mixtures thereof.

Claim 10

Dependent Claim 12 words

The method of claim 1 wherein the silicate is a cyclic silicate.

Claim 11

Dependent Claim 51 words

The method of claim 9 wherein the silicate is selected. from the group consisting of Ca 3 Si 3 O 9 , M1(Pb 2 g)(Si 4 O 12 ) Cu 6 Si 6 O 18 .6H 2 O and Na 4 Ca 4 Si 6 O 18 , or mixtures thereof.

Claim 12

Dependent Claim 65 words

The method of claim 9 wherein the cyclic silicate contains the ion [Si 6 O 18 ] 12- and is prepared by the steps of: (a) mixing sources of Na 1+ , Ca 2+ , Si 4+ and O 2+ ; and (b) calcining the resulting mixture at a temperature of at least about 1000° C. until [Si 6 O 18 ] 12- is formed.

Claim 13

Dependent Claim 12 words

The method of claim 1 wherein the alcohol contains 1-8 carbon atoms.

Claim 14

Dependent Claim 25 words

The method of claim 12 wherein the alcohol is selected from the group consisting of methanol, ethanol, n-propanol, isopropanol, n-butanol and sec-butanol, or mixtures thereof.

Claim 15

Dependent Claim 49 words

The method of claim 1 wherein the mixture of silicate with acid in alcohol solution is heated and byproduct water is removed as a distillate component, the product is extracted from the distillation residue using an organic solvent, and the product is then isolated by distillation of the solvent.

Claim 16

Dependent Claim 53 words

The method of claim 1 wherein the mixture of silicate with acid in alcohol solution is added to a distilling alcohol and byproduct water is removed as a distillate component, the product is extracted from the distillation residue using an organic solvent, and the product is then isolated by distillation of the solvent.

Claim 17

Dependent Claim 12 words

The method of claim 1 wherein the acid is a strong acid.

Claim 18

Dependent Claim 25 words

The method of claim 1 wherein the acid is selected from the group consisting of hydrochloric, hydrobromic, sulfuric, phosphoric, and oxalic acids, or mixtures thereof.

Claim 19

Dependent Claim 11 words

The method of claim 1 wherein the acid is hydrochloric acid.

Claim 20

Dependent Claim 31 words

The method of claim 1 wherein organosilanes and organosiloxanes are prepared by the additional steps of reacting the product alkoxysilanes and alkoxysiloxanes with an alkylating agent and recovering organosilanes and organosiloxanes.

Claim 21

Dependent Claim 21 words

The method of claim 19 wherein the alkylating agent is selected from the group consisting of Grignard reagents and organolithium reagents.

Claim 22

Dependent Claim 23 words

The method of claim 19 wherein the organosilanes and organosiloxanes are recovered by extraction and separation steps using pentane and aqueous hydrochloric acid.

Claim 23

Independent Claim 95 words

A method for preparing alkoxysilanes and alkoxysiloxanes which comprises the steps of: (a) suspending a finely divided silicate in a C 1-8 alcohol; (b) contacting the suspension of (a) with a solution of anhydrous or aqueous hydrochloric acid in a C 1-8 alcohol while maintaining the temperature below about 25° C.; (c) introducing the mixture formed in (b) slowly into distilling alcohol and simultaneously stripping out low boiling components and byproduct water by distillation; (d) extracting the residue after distillation with an organic solvent; and (e) concentrating the solvent extract of (d) to isolate product.

Claim 24

Independent Claim 95 words

A method for preparing alkoxysilanes and alkoxysiloxanes which comprises the steps of: (a) suspending a finely divided silicate in a C 1-8 alcohol; (b) contacting the suspension of (a) with a solution of anhydrous or aqueous hydrochloric acid in a C 1-8 alcohol while maintaining the temperature below about 25° C.; (c) introducing the mixture formed in (b) slowly into distilling alcohol and simultaneously stripping out low boiling components and byproduct water by distillation; (d) extracting the residue after distillation with an organic solvent; and (e) concentrating the solvent extract of (d) to isolate product.

Claim 25

Dependent Claim 14 words

The method of claim 22 wherein the alcohol of (a) and (b) is ethanol.

Claim 26

Dependent Claim 29 words

The method of claim 22 wherein the amount of hydrochloric acid used in (b) is sufficient to displace all or nearly all of the metal ions of the silicate.

Claim 27

Dependent Claim 19 words

The method of claim 22 wherein toluene is added to (c) and byproduct water is removed by azeotropic distillation.

Claim 28

Dependent Claim 13 words

The method of claim 22 wherein the organic solvent of (d) is pentane.

Claim 29

Dependent Claim 12 words

The method of claim 22 wherein the concentration step (e) is distillation.

Claim 30

Dependent Claim 81 words

The method of claim 22 wherein organosilanes and organosiloxanes are prepared by including the additional steps of: (f) preparing a solution of the product alkoxysilanes and alkoxysiloxanes from (e) in an ether; (g) adding to the solution of (f) a mixture of alkylating agent in an ether; (h) maintaining the resulting reaction mixture at a temperature up to the boiling point of the ether until organosilanes and organosiloxanes are formed; and (i) concentrating the mixture and recovering the organosilanes and organosiloxanes.

Claim 31

Dependent Claim 14 words

The method of claim 28 wherein the ether of (f) and (g) is tetrahydrofuran.

Claim 32

Dependent Claim 13 words

The method of claim 28 wherein the alkylating agent is a Grignard reagent.

Claim 33

Dependent Claim 23 words

The method of claim 28 wherein the organosilanes and organosiloxanes are recovered by extraction and separation steps using pentane and aqueous hydrochloric acid.

Claim 34

Independent Claim 58 words

A method for preparing the cyclic silicate ion [Si 6 O 18 ] 12- which comprises mixing silica and compounds selected from the alkali metal carbonates and the alkaline earth metal carbonates, or mixtures thereof, and calcining the resulting mixture at a temperature of at least about 1000° C. until [Si 6 O 18 ] 12- is formed.

Claim 35

Independent Claim 58 words

A method for preparing the cyclic silicate ion [Si 6 O 18 ] 12- which comprises mixing silica and compounds selected from the alkali metal carbonates and the alkaline earth metal carbonates, or mixtures thereof, and calcining the resulting mixture at a temperature of at least about 1000° C. until [Si 6 O 18 ] 12- is formed.

Claim 36

Dependent Claim 3 words

The compound dodecaethoxycyclohexasiloxane.

Claim 37

Dependent Claim 3 words

The compound dodecaethoxycyclohexasiloxane.

Claim 38

Dependent Claim 3 words

The compound decaethoxybicyclo[5.5.1]-hexasiloxane.

Claim 39

Dependent Claim 3 words

The compound decaethoxybicyclo[5.5.1]-hexasiloxane.

Claim 40

Dependent Claim 3 words

The compound decaethoxybicyclo[5.3.3]-hexasiloxane.

Claim 41

Dependent Claim 3 words

The compound decaethoxybicyclo[5.3.3]-hexasiloxane.

Claim 42

Dependent Claim 6 words

The compound octaethoxytricyclo[5.5.1.1 3 ,9 ]-hexasiloxane.

Claim 43

Dependent Claim 6 words

The compound octaethoxytricyclo[5.5.1.1 3 ,9 ]-hexasiloxane.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1991-01-04	1991-07-06	1992-01-05	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1995-01-04	1995-07-06	1996-01-05	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	1999-01-04	1999-07-06	2000-01-05	$7700.00	Window Closed / Lapsed

Silicate esters and organosilicon compounds

Abstract

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