Palladium/alumina catalyst and preparation method thereof

Abstract

The invention discloses a preparation method of a sulfuration mode Pd / Al2O3 catalyst. The method comprises the following steps: 1, preparing a sodium alkyl xanthate solution and a palladium-containing dipping liquid which is acidic; 2, dipping an alumina carrier in the palladium-containing dipping liquid, filtering, drying, spraying parts of the palladium-containing dipping liquid, and drying to obtain a catalyst intermediate; and 3, adding the catalyst intermediate to the remaining palladium-containing dipping liquid, dipping, drying, and roasting to obtain the sulfuration mode Pd / Al2O3 catalyst. A volume ratio of the palladium-containing dipping liquid used for spraying to the palladium-containing dipping liquid used for dipping is 1.0:1.0-1.0:3.0, and preferably 1.0:1.5-1.0:2.5. The catalyst obtained through the method realizes higher activity, higher selectivity and longer life than present catalysts prepared through present methods in the synthesis process of methyl isobutyl ketone from acetone.

Description

technical field

[0001] The invention relates to a preparation method of a sulfide-type palladium / alumina catalyst, in particular to a preparation method of a catalyst for synthesizing methyl isobutyl ketone from acetone. Background technique

[0002] Methyl isobutyl ketone (MIBK for short) is an important organic solvent, mainly used in paint, resin coating, waxy oil dewaxing, and also one of the raw materials for the production of rubber antioxidant 4020, with a wide range of uses.

[0003] The traditional production method is a three-step method, which has problems such as polluting the environment, high production costs, and complicated processes, and has been gradually eliminated. The one-step method is the most advanced technology for synthesizing methyl isobutyl ketone from acetone. This technology requires that the catalyst must have a dual-functional active center, that is, a condensation dehydration acid center and a hydrogenation active center.

[0004] The Pd / res...

Examples

Embodiment 1

[0024] (1) Preparation of impregnation solution

[0025] (a) put sodium ethyl xanthate in a 200ml beaker, add deionized water to dissolve, and prepare a solution containing 0.5wt% sodium ethyl xanthate; (b) add Pd(NO 3 ) 2 2H 2 O was put in a 200 ml beaker, dissolved in deionized water, adjusted to pH 4 with nitric acid, and prepared as an impregnating solution containing 0.15 wt% palladium.

[0026] (2) Loading vulcanized active components Measure 11ml of a solution containing 0.5wt% sodium ethyl xanthate and pour it into a 100ml beaker, take 10g of γ-alumina (specific surface area 189m 2 / g, pore volume 0.4mL / g) was poured into it, immersed for 3 hours, filtered, and dried at 100°C for 2 hours to obtain a dry sample. Measure 14 ml of impregnation solution containing palladium 0.15wt% and spray dry the sample at 115°C After drying for 6 hours, a catalyst intermediate was obtained.

[0027] (3) Loaded oxidized active components

[0028] Measure 23 ml of impregnation sol...

Embodiment 2

[0030] (1) (a) put sodium propyl xanthate in a 200 ml beaker, add deionized water to dissolve, and prepare a solution containing 0.5wt% sodium propyl xanthate; step (b) is the same as in Example 1 ( b).

[0031](2), loaded vulcanized active components

[0032] Measure 10 milliliters of 0.5wt% sodium propyl xanthate solution and pour it into a 100 milliliter beaker, take 10 grams of γ-alumina (specific surface area 189m 2 / g, pore volume 0.4mL / g) was poured into it, soaked for 4 hours, filtered, and dried at 105°C for 3 hours to obtain a dry sample. Measure 10ml of impregnation solution containing palladium 0.15wt% and spray dry the sample at 115°C After drying for 6 hours, a catalyst intermediate was obtained.

[0033] (3) Loaded oxidized active components

[0034] Measure 17 ml of impregnating solution containing 0.15 wt% palladium in a 200 ml beaker, pour the catalyst intermediate obtained in step (2) into it, routinely impregnate for 3 hours, filter, dry at 105°C for...

Embodiment 3

[0036] (1) Same as embodiment 1

[0037] (2) Loaded vulcanized active components

[0038] Measure 6 milliliters of a solution containing 0.5 wt % sodium ethyl xanthate and pour it into a 100 milliliter beaker, take 10 g of γ-alumina (specific surface area 189m 2 / g, pore volume 0.4mL / g) was poured into it, soaked for 4 hours, filtered, and dried at 105°C for 2 hours to obtain a dry sample. Measure 6 ml of impregnation solution containing palladium 0.15wt% and spray dry the sample at 115°C Dry for 6 hours to obtain a catalyst intermediate;

[0039] (3) Loaded oxidized active components

[0040] Measure 14 ml of impregnation solution containing 0.15 wt% palladium in a 200 ml beaker, pour the catalyst intermediate obtained in step (2) into it, impregnate it for 5 hours, filter, dry at 105°C for 6 hours, and roast at 450°C for 6 hours hours, the finished catalyst M-3 was obtained, and the amount of palladium loaded on the catalyst was 0.30wt%.

technical field

[0001] The invention relates to a preparation method of a sulfide-type palladium / alumina catalyst, in particular to a preparation method of a catalyst for synthesizing methyl isobutyl ketone from acetone. Background technique

[0002] Methyl isobutyl ketone (MIBK for short) is an important organic solvent, mainly used in paint, resin coating, waxy oil dewaxing, and also one of the raw materials for the production of rubber antioxidant 4020, with a wide range of uses.

[0003] The traditional production method is a three-step method, which has problems such as polluting the environment, high production costs, and complicated processes, and has been gradually eliminated. The one-step method is the most advanced technology for synthesizing methyl isobutyl ketone from acetone. This technology requires that the catalyst must have a dual-functional active center, that is, a condensation dehydration acid center and a hydrogenation active center.

[0004] The Pd / res...

Examples

Embodiment 1

[0024] (1) Preparation of impregnation solution

[0025] (a) put sodium ethyl xanthate in a 200ml beaker, add deionized water to dissolve, and prepare a solution containing 0.5wt% sodium ethyl xanthate; (b) add Pd(NO 3 ) 2 2H 2 O was put in a 200 ml beaker, dissolved in deionized water, adjusted to pH 4 with nitric acid, and prepared as an impregnating solution containing 0.15 wt% palladium.

[0026] (2) Loading vulcanized active components Measure 11ml of a solution containing 0.5wt% sodium ethyl xanthate and pour it into a 100ml beaker, take 10g of γ-alumina (specific surface area 189m 2 / g, pore volume 0.4mL / g) was poured into it, immersed for 3 hours, filtered, and dried at 100°C for 2 hours to obtain a dry sample. Measure 14 ml of impregnation solution containing palladium 0.15wt% and spray dry the sample at 115°C After drying for 6 hours, a catalyst intermediate was obtained.

[0027] (3) Loaded oxidized active components

[0028] Measure 23 ml of impregnation sol...

Embodiment 2

[0030] (1) (a) put sodium propyl xanthate in a 200 ml beaker, add deionized water to dissolve, and prepare a solution containing 0.5wt% sodium propyl xanthate; step (b) is the same as in Example 1 ( b).

[0031](2), loaded vulcanized active components

[0032] Measure 10 milliliters of 0.5wt% sodium propyl xanthate solution and pour it into a 100 milliliter beaker, take 10 grams of γ-alumina (specific surface area 189m 2 / g, pore volume 0.4mL / g) was poured into it, soaked for 4 hours, filtered, and dried at 105°C for 3 hours to obtain a dry sample. Measure 10ml of impregnation solution containing palladium 0.15wt% and spray dry the sample at 115°C After drying for 6 hours, a catalyst intermediate was obtained.

[0033] (3) Loaded oxidized active components

[0034] Measure 17 ml of impregnating solution containing 0.15 wt% palladium in a 200 ml beaker, pour the catalyst intermediate obtained in step (2) into it, routinely impregnate for 3 hours, filter, dry at 105°C for...

Embodiment 3

[0036] (1) Same as embodiment 1

[0037] (2) Loaded vulcanized active components

[0038] Measure 6 milliliters of a solution containing 0.5 wt % sodium ethyl xanthate and pour it into a 100 milliliter beaker, take 10 g of γ-alumina (specific surface area 189m 2 / g, pore volume 0.4mL / g) was poured into it, soaked for 4 hours, filtered, and dried at 105°C for 2 hours to obtain a dry sample. Measure 6 ml of impregnation solution containing palladium 0.15wt% and spray dry the sample at 115°C Dry for 6 hours to obtain a catalyst intermediate;

[0039] (3) Loaded oxidized active components

[0040] Measure 14 ml of impregnation solution containing 0.15 wt% palladium in a 200 ml beaker, pour the catalyst intermediate obtained in step (2) into it, impregnate it for 5 hours, filter, dry at 105°C for 6 hours, and roast at 450°C for 6 hours hours, the finished catalyst M-3 was obtained, and the amount of palladium loaded on the catalyst was 0.30wt%.