Claims
- 1. In a process for preparing a compound of the formula H.sub.x.sub.+1 Si (OR).sub.4.sub.-x.sub.-1 or one of the formula H.sub.x.sub.-1 Si (OR).sub.4.sub.-x.sub.+1 wherein R is alkyl or alkoxyalkyl wherein the alkyl portion has up to 10 carbon atoms and x equals 1, 2 or 3 by reacting a compound of the formula H.sub.x Si (OR).sub.4.sub.-x in the presence of a catalyst under distillation conditions, distilling over and recovering a product of the formula H.sub.x.sub.+1 Si (OR).sub.4.sub.-x.sub.-1 or a product of the formula H.sub.x.sub.-1 Si (OR).sub.4.sub.-x.sub.+1, the improvement which comprises utilizing as the catalyst an oxide, halide, chloride, carbonate, acetate, ethylate or acetyl acetonate of zinc, cadmium, magnesium, calcium, strontium or barium, metallic zinc, metallic cadmium, metallic calcium, metallic magnesium, metallic strontium or metallic barium or metallic manganese or manganese chloride, manganese carbonate or zinc, aluminum or manganese acetylacetonate or an organic nitrogen compound selected from the group consisting of primary C.sub.1 -C.sub.8 alkylamines, secondary C.sub.1 -C.sub.8 alkylamines, tertiary C.sub.1 -C.sub.8 alkylamines, substituted carboxylic acid amides of C.sub.1 -C.sub.8 alkanoic acid amides, amides of phoshoric acid, pyridine, quinoline, isoquinoline and piperidine.
- 2. A process according to claim 1 wherein the catalyst is in the form of a compound.
- 3. A process according to claim 1 wherein the catalyst is an element in metallic form.
- 4. In a process for preparing a compound of the formula H.sub.x.sub.+1 Si (OR).sub.4.sub.-x.sub.-1 or one of the formula H.sub.x.sub.-1 Si (OR).sub.4.sub.-x.sub.+1 wherein R is alkyl or alkoxy alkyl wherein the alkyl portion has up to 10 carbon atoms and x equals 1, 2 or 3 by reacting a compound of the formula H.sub.x Si (OR).sub.4.sub.-x in the presence of a catalyst under distillation conditions, distilling over and recovering a product of the formula H.sub.x.sub.+1 Si (OR).sub.4.sub.-x.sub.-1 or a product of the formula H.sub.x.sub.-1 Si (OR).sub.4.sub.-x.sub.+1 which comprises utilizing as the catalyst a catalyst selected from the group consisting of lithium hydroxide, lithium oxide, lithium carbonate, lithium phosphate, lithium halide, sodium bicarbonate, cesium oxide, sodium silicate, sodium borate, magnesium oxide, magnesium halide, magnesium carbonate, magnesium acetate, magnesium ethylate, magnesium acetylacetonate, metallic magnesium, metallic calcium, metallic strontium, metallic barium, an oxide, halide, hydroxide, carbonate, acetate or acetylacetonate of calcium, strontium or barium, metallic aluminum, metallic lanthanum, metallic cerium, metallic thorium, metallic uranium, metallic iron, FeSO.sub.4, iron acetylacetonate, manganese chloride, manganese metal, manganese carbonate, manganese acetylacetonate, manganese sulfate, aluminum acetylacetonate, zinc acetylacetonate, primary C.sub.1 -C.sub.8 alkyl amines, secondary C.sub.1 -C.sub.8 alkyl amines, tertiary C.sub.1 -C.sub.8 alkyl amines, a C.sub.1 -C.sub.8 alkanoic acid amine, an amide of phosphoric acid, pyridine, quinoline, isoquinoline and piperidine.
- 5. A process according to claim 4 wherein the catalyst is a C.sub.1 -C.sub.8 alkyl amine a phosphoric acid amide or a C.sub.1 -C.sub.8 alkanoic acid amide, said amine or amide is a composition selected from the group consisting of urea, dimethylformamide, diethylformamide and hexamethylene phosphoric acid triamide.
- 6. A process according to claim 1 wherein the catalyst is present in the reaction mixture in the form of a solid.
- 7. A process according to claim 1 wherein the catalyst is present in the reaction mixture in the form of a suspension.
- 8. A process according to claim 1 wherein the catalyst is present in a water-free dissolved form.
- 9. A process according to claim 1 wherein the reaction mixture is held at a temperature of between 10.degree. and 0.degree. C from the boiling point during distillative removal of the desired reaction product.
- 10. A process according to claim 1 wherein after said compound having the formula H.sub.x Si (OR).sub.4.sub.-x or H.sub.x.sub.+1 Si (OR).sub.4.sub.-x.sub.-1 or H.sub.x.sub.-1 Si (OR).sub.4.sub.-x.sub.+1 is removed, the reaction mixture is heated up to a higher temperature at which point a compound of the formula H.sub.x.sub.+1 Si (OR).sub.4.sub.-x.sub.-1 or H.sub.x.sub.-1 Si (OR).sub.4.sub.-x.sub.+1 is removed by distillation.
- 11. A process according to claim 1 wherein the compound reacted is a trialkoxysilane.
- 12. A process according to claim 1 wherein R is an alkyl group of up to 10 carbon atoms or an alkyl alkoxy group having up to 10 carbon atoms on the alkoxy group and up to 10 carbon atoms on the alkyl group.
- 13. A process according to claim 4 wherein the catalyst is magnesium acetylacetonate.
- 14. A process according to claim 4 wherein the catalyst is hexamethyl phosphoric acid triamide.
- 15. A process according to claim 4 wherein the catalyst is iron(II)-acetylacetonate.
- 16. A process according to claim 4 wherein the catalyst is aluminum acetylacetonate.
- 17. A process according to claim 4 wherein the catalyst is zinc acetylacetonate.
- 18. A process according to claim 1 wherein the compound reacted is trimethoxysilane.
- 19. A process according to claim 1 wherein the compound reacted is triethoxysilane.
- 20. A process according to claim 1 wherein the compound reacted is di-(2-methoxyethoxy)-silane.
- 21. A process according to claim 1 wherein the distillation is carried out such that the return ratio is between 1 and 100.
- 22. A process according to claim 4 wherein the catalyst is selected from the group consisting of magnesium oxide, magnesium halide, magnesium carbonate, magnesium acetate, magnesium ethylate, magnesium acetylacetonate, metallic magnesium, metallic calcium, metallic strontium, metallic barium, an oxide, halide, hydroxide, carbonate, acetate or acetylacetonate of calcium, strontium or barium metallic aluminum, metallic lanthanum, metallic cerium, metallic thorium, metallic uranium, metallic iron, FeSO.sub.4, iron acetylacetonate. primary C.sub.1 -C.sub.8 alkyl amines, secondary C.sub.1 -C.sub.8 alkyl amines, tertiary C.sub.1 -C.sub.8 alkyl amines, a C.sub.1 -C.sub.8 alkanoic acid amide, pyridine, quinoline, isoquinoline and piperidine.
- 23. A process according to claim 4 wherein the catalyst is lithium chloride.
- 24. A process according to claim 4 wherein the catalyst is magnesium chloride.
- 25. A process according to claim 22 wherein the catalyst is selected from the group consisting of magnesium oxide, magnesium halide, magnesium carbonate, magnesium acetate, magnesium ethylate, magnesium acetylacetonate, metallic magnesium, metallic calcium, metallic strontium, metallic barium, an oxide, hydroxide, carbonate, acetate or acetylacetonate of calcium, strontium or barium, metallic aluminum, metallic lanthanum, metallic cerium, metallic thorium, metallic uranium, metallic iron, FeSO.sub.4, iron acetylacetonate, primary C.sub.1 -C.sub.8 alkyl amines, secondary C.sub.1 -C.sub.8 alkyl amines, tertiary C.sub.1 -C.sub.8 alkyl amines, a C.sub.1 -C.sub.8 alkanoic acid amide, pyridine, quinoline, isoquinoline and piperidine.
Priority Claims (1)
Number |
Date |
Country |
Kind |
2226265 |
May 1972 |
DT |
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CROSS REFERENCE TO RELATED APPLICATION
This is a continuation-in-part of application Ser. No. 360,486 filed May 15, 1973, now abandoned.
US Referenced Citations (5)
Continuation in Parts (1)
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Number |
Date |
Country |
Parent |
360486 |
May 1973 |
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