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A kind of preparation method of sulfurized palladium/alumina catalyst

A catalyst and alumina technology, which is applied in the preparation of organic compounds, catalysts for physical/chemical processes, carbon-based compounds, etc., can solve the problems of affecting device operation efficiency, complicated process, high operating costs, etc., to achieve extended operation period, The preparation process is simple and the life extension effect

Active Publication Date: 2016-02-10
CHINA PETROLEUM & CHEM CORP +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

[0023] a. Preparation of impregnation solution

[0024] Pd(NO 3 ) 2 2H 2 O is placed in a 200 ml beaker, dissolved in deionized water, adjusted to pH 4 with nitric acid, and prepared as an impregnation solution containing 0.25 wt% palladium.

[0025] Put the sodium ethyl xanthate in a 200 ml beaker, add deionized water to dissolve, and prepare a solution containing 0.5 wt % of the sodium ethyl xanthate.

[0026] b. Loading active components

[0027] Catalyst design loading palladium amount 0.5wt%, measure 20 milliliters of impregnating solution containing palladium 0.25wt% in 200 milliliter beaker, get 10g gamma-alumina carrier (specific surface area 189m 2 / g, pore volume 0.4mL / g, strip. ) into it, put the beaker in a water bath, heat at 65°C, soak for 3 hours, then add dropwise 10 ml of a solution containing 0.5wt% sodium ethyl xanthate, the molar ratio of sodium ethyl xanthate to palladium The ratio is 0.74:1, the impregnation time is 3 hours, the residual liquid is r...

Embodiment 2

[0029] a. Preparation of impregnation solution

[0030] Pd(NO 3 ) 2 2H 2 O is placed in a 200 ml beaker, dissolved in deionized water, adjusted to pH 3 of the impregnation solution with nitric acid, and prepared into an impregnation solution containing 0.25 wt% palladium.

[0031] Put sodium propyl xanthate in a 200 ml beaker, add deionized water to dissolve, and prepare a solution containing 0.5 wt% sodium propyl xanthate.

[0032] b. Loading active components

[0033] Catalyst design loading palladium amount 0.4wt%, measure 16 milliliters of impregnating solution containing palladium 0.25wt% in 200 milliliter beaker, get 10g gamma-alumina carrier (property is the same as embodiment 1) and pour it into it, put the beaker in the water bath, Heating at 70°C, soaking for 3 hours, then adding dropwise 8 ml of a solution containing 0.5wt% sodium propyl xanthate and palladium, the molar ratio of sodium propyl xanthate to palladium is 0.68:1, soaking for 4 hours, filtering to re...

Embodiment 3

[0035] a, with embodiment 1

[0036] b. Loading active components

[0037]The palladium loading amount of the catalyst design is 0.3wt%, measure 12 milliliters of impregnation solution containing palladium 0.25wt% in a 200 milliliter beaker, get 10g gamma-alumina carrier (the property is the same as embodiment 1) and pour it into it, put the beaker in a water bath, heat Temperature at 65°C, soak for 4 hours, then add dropwise 5 ml of a solution containing 0.5wt% sodium ethyl xanthate, the molar ratio of sodium ethyl xanthate to palladium is 0.6:1, soak for 4 hours, filter to remove the residual solution , dried at 105°C for 6 hours, and calcined at 450°C for 7 hours to obtain the finished catalyst M-3.

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Abstract

The invention discloses a preparation method for a sulfuration palladium / alumina catalyst. The method comprises the following steps: preparing an acidic impregnating solution containing palladium and impregnating an alumina carrier in the impregnating solution containing palladium for a certain period of time; then adding a proper amount of a sodium alkyl xanthate solution drop by drop; and carrying out filtering, drying and roasting after completion of impregnation so as to obtain the sulfuration palladium / alumina catalyst. The method provided by the invention overcomes the disadvantage of mismatching between a hydrogenation function and a condensation dehydration function of conventional oxidized palladium / alumina catalysts for synthesis of methyl isobutyl ketone from acetone, and when used for synthesis of methyl isobutyl ketone from acetone, the prepared catalyst has superior reaction activity than catalysts used in conventional processes.

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 water, mainly used for dewaxing of paints, resin coatings, and waxy oils. It is also one of the raw materials for the production of rubber antioxidant 4020, and has 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 ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/045C07C45/73C07C49/04
Inventor 宋丽芝乔凯王海波勾连科薛冬
Owner CHINA PETROLEUM & CHEM CORP
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