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A kind of sulfurized palladium/alumina catalyst and its preparation method and application

A catalyst and vulcanization-type technology, which is applied in the field of acetone synthesis methyl isobutyl ketone catalyst and its preparation, can solve the problems of long vulcanization time, complicated process, and affecting the operation efficiency of the device.

Active Publication Date: 2017-02-01
中石化(大连)石油化工研究院有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process is complicated, the vulcanization time is long, and the operating cost is high, which affects the operating efficiency of the device.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Preparation of impregnation solution

[0026] (a) put palladium ethyl xanthate in a 200 ml beaker, add acetone to dissolve, and prepare an organic impregnation solution containing 0.15wt% palladium; (b) add Pd(NO 3 ) 2 2H 2 O is put in the 200 milliliter beaker, adds deionized water to dissolve, adjusts the impregnation solution pH value to 4 with nitric acid, is mixed with the inorganic palladium salt impregnation solution containing palladium 0.2wt%.

[0027] (2) Loaded vulcanized active components

[0028] Measure 13 milliliters of ethyl xanthate palladium solution containing palladium 0.15wt% and pour it into a 50 milliliter beaker, get 10 g gamma-alumina (specific surface area 189m 2 / g, pore volume 0.4mL / g) was poured into it, impregnated for 3 hours, filtered, and dried at 100°C for 2 hours to obtain a dry catalyst intermediate. The supported palladium accounted for the final Pd / Al 2 o 3 39% of the total weight of palladium in the catalyst.

[0029] (3)...

Embodiment 2

[0032] (1) (a) Put palladium propyl xanthate in a 200 ml beaker, add acetone to dissolve, and prepare an organic impregnation solution containing 0.15 wt% palladium; step (b) is the same as in Example 1 (b).

[0033] (2) Loaded vulcanized active components

[0034] Measure 10 milliliters of propyl xanthate palladium solution containing palladium 0.15wt% and pour it into a 50 milliliter beaker, get 10 g gamma-alumina (specific surface area 189m 2 / g, pore volume 0.4mL / g) was poured into it, impregnated for 4 hours, filtered, and dried at 105°C for 3 hours to obtain a dry catalyst intermediate. The supported palladium accounted for the final Pd / Al 2 o 3 36% of the total weight of palladium in the catalyst.

[0035] (3) Loaded oxidized active components

[0036] Measure 13.5 ml of impregnating solution of inorganic palladium salt containing palladium 0.2wt% in a 50 ml beaker, pour the catalyst intermediate obtained in step (2) into it, impregnate for 5 hours, filter, dry at 10...

Embodiment 3

[0038] (1) Same as embodiment 1

[0039] (2) Loading vulcanization-type active components Measure 7ml of palladium ethyl xanthate solution containing 0.15wt% palladium and pour it into a 50ml beaker, take 10g of γ-alumina (specific surface area 189m 2 / g, pore volume 0.4mL / g) was poured into it, impregnated for 4 hours, filtered, and dried at 105°C for 2 hours to obtain a dry catalyst intermediate. The supported palladium accounted for the final Pd / Al 2 o 3 35% of the total weight of palladium in the catalyst.

[0040] (3) Loaded oxidized active components

[0041] Measure 9.8 ml of the impregnating solution of inorganic palladium salt containing palladium 0.2wt% in a 50 ml beaker, pour the catalyst intermediate obtained in step (2) into it, routinely impregnate for 5 hours, filter, and dry at 105°C for 6 hours. ℃ roasting for 6 hours to obtain the finished catalyst M-3, the total palladium weight content of the catalyst is 0.3%.

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Abstract

The invention discloses a preparation method of a sulfuration mode Pd / Al2O3 catalyst. The method comprises the following steps: 1, preparing a palladium alkyl xanthate solution and an inorganic palladium salt-containing dipping liquid which is acidic; 2, dipping an alumina carrier in the palladium alkyl xanthate solution, filtering, and drying to obtain a catalyst intermediate; and 3, adding the catalyst intermediate to the inorganic palladium salt-containing dipping liquid, dipping, drying, and roasting to obtain the sulfuration mode Pd / Al2O3 catalyst. Palladium supported in step 2 accounts for 20-40wt% of total palladium (by palladium element) in the finished Pd / Al2O3 catalyst. 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 sulfide-type palladium / alumina catalyst and its preparation method and application, in particular to a catalyst for synthesizing methyl isobutyl ketone from acetone and its preparation method and application. 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 hydrogenati...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44C07C45/74C07C49/04
Inventor 宋丽芝王海波勾连科薛冬
Owner 中石化(大连)石油化工研究院有限公司
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