2-hydroxyethyl 2-oxo-1,3-dioxolane-4-carboxylates, their preparation and use
US-10059685-B2 · Aug 28, 2018 · US
US9834536B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-9834536-B2 |
| Application number | US-201414786334-A |
| Country | US |
| Kind code | B2 |
| Filing date | Apr 22, 2014 |
| Priority date | Apr 23, 2013 |
| Publication date | Dec 5, 2017 |
| Grant date | Dec 5, 2017 |
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A method for producing a heterogeneous catalyst for use of synthesizing cyclic carbonates by reacting an epoxide and carbon dioxide in the presence of the catalyst. A method for making a catalyst that includes forming a catalyst precursor then reacting the catalyst precursor with a tertiary phosphine.
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The invention claimed is: 1. A method for producing a catalyst, comprising: obtaining a catalyst precursor having a haloalkyl group or a haloaryl group, by reacting a silane compound having a haloalkyl group or a haloaryl group with a silica gel having an average pore diameter of 3.5 nm to 50 nm, and obtaining the catalyst, by reacting the catalyst precursor with a tertiary phosphine, at a temperature of 100-160° C. for 10-50 hours in xylene, wherein the catalyst formed by the reacting has a [halogen]/[phosphorus] molar ratio of 0.8 to 1.5, wherein the catalyst has a phosphorus content of 0.25 mmol to 0.6 mmol per 1 g of the catalyst, wherein the silane compound has formula (1): X—R 1 —Si(OR 2 ) 3 (1) wherein R 1 represents a linear or branched alkylene group having 2 to 8 carbon atoms, an arylene group, an alkarylene group, an arylenealkylene group or an alkylenearylene group; R 2 represents an alkyl group having 1 to 4 carbon atoms; and X represents a halogen atom, and wherein the tertiary phosphine has formula (2): wherein R 3 to R 5 each independently represents an alkyl group having 1 to 8 carbon atoms, an aryl group, an aralkyl group, an alkoxyalkyl group or an alkoxy substituted aryl group. 2. The method according to claim 1 , wherein the silica gel has an average pore diameter of 3.5 nm to 25 nm. 3. The method according to claim 1 , wherein the [halogen]/[phosphorus] molar ratio is 1.0 to 1.5. 4. The method according to claim 1 , wherein the catalyst obtained has a specific surface area of 100 m 2 /g to 1,000 m 2 /g. 5. The method according to claim 1 , wherein the silica gel has an average pore diameter of 10 nm to 25 nm. 6. The method according to claim 1 , wherein the catalyst has a surface area of from 80 to 273 m 2 /g. 7. The method according to claim 1 , wherein the catalyst obtained has a phosphorus content of 0.3 to 0.56 mmol per 1 g of the catalyst. 8. The method according to claim 1 , further comprising: forming the silica gel, before obtaining the catalyst precursor, by treating the silica gel with hydrochloric acid then washing with water. 9. The method according to claim 1 , wherein the [halogen]/[phosphorus] molar ratio is 0.8 to 1.4. 10. The method according to claim 1 , wherein the [halogen]/[phosphorus] molar ratio is 0.8 to 1.3.
Operations & Transport · mapped topic
on mineral substrates · CPC title
Operations & Transport · mapped topic
Halogen-containing compounds · CPC title
Phosphonium compounds, i.e. phosphine with an additional hydrogen or carbon atom bonded to phosphorous so as to result in a formal positive charge on phosphorous · CPC title
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