Vapor-phase carbonylation of lower alkyl alcohols using tungsten promoted group VIII catalyst
A technology of carbonylation and catalyst, applied in organic chemistry, organic chemical methods, carbon monoxide reaction to prepare carboxylic acid, etc., can solve problems such as not suitable for vapor phase process, unstable catalyst, etc.
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment
[0055] Catalyst 1
[0056] In preparing the catalyst, 579 milligrams (mg) of hexachloroplatinic acid having a Pt assay of 39.23% (1.17 mmol Pt) was dissolved in 30 milliliters (mL) of distilled water. This solution was then added to 20.0 grams of 12 x 40 mesh activated carbon pellets (available from Calgon) packed in an evaporating dish. The BET surface area of activated carbon granules exceeds 800m 2 / g. The mixture is dried using a steam bath with continuous stirring until the carrier granules become free flowing. The impregnated catalyst was then transferred to a quartz tube measuring 106 cm long x 25 mm outer diameter. The quartz tube was then placed in a three-element electric tube furnace with the mixture in the approximate center of the furnace's 61 cm long heating zone. Nitrogen was continuously flowed through the catalyst bed at a rate of 100 sccm / min. The tube was heated from room temperature to 300°C over 2 hours, held at 300°C for 2 hours and then cooled bac...
Embodiment II
[0060] The second catalyst was prepared by dissolving 0.331 g of ammonium tungstate (1.17 mmol) in 30 mL of distilled water heated to 50° C. to completely dissolve the ammonium tungstate. This solution was then added to 20.0 grams of 12 x 40 mesh activated carbon pellets (available from Calgon) packed in an evaporating dish. The BET surface area of activated carbon granules exceeds 800m 2 / g. The mixture was then dried as described above in Example 1 and placed in a quartz tube.
[0061] A second solution was prepared by dissolving 0.207 grams of palladium chloride (1.16 mmol of Pd) in 15 mL of distilled water and 15 mL of 11.6M HCl. It was subsequently added to the tungsten impregnated catalyst prepared above. The mixture was reheated with continuous stirring using a steam bath until the granules became free flowing and then transferred to a quartz tube as described above.
[0062] The solid supported catalyst according to the invention (Catalyst 2) has a density of 0.5...
Embodiment 1
[0089] The compositions and weights of samples taken periodically during the above procedure in which Catalyst 1 was used are given in Table 1, where "time" is the total time in hours of the carbonylation operation from the start of methanol addition until the time a particular sample was taken . The values given below for "MeI" (methyl iodide), "MeOAc" (methyl acetate), "MeOH" (methanol) and "HOAc" (acetic acid) are weight percents of each compound present in the samples. The weight of each sample is given in grams.
[0090] Number of samples
time elapsed
(h)
MeI
(Wt.%)
MeOAc
(Wt.%)
MeOH
(Wt.%)
HOAc
(Wt.%)
(g)
1
3.5
16.11
35.79
19.73
15.46
46.2
2
5.5
15.99
36.48
19.89
15.37
29.8
3
8.5
16.15
36.43
19.72
15.27
30.9
4
10.5
17.97
31.22
...
PUM
| Property | Measurement | Unit |
|---|---|---|
| density | aaaaa | aaaaa |
| boiling point | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More