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Preparation method for sulfuration palladium/alumina catalyst

A catalyst and vulcanization-type technology, which is applied in the field of preparation of methyl isobutyl ketone catalyst for the synthesis of acetone, can solve the problems of affecting the operation efficiency of the device, complicated process, long vulcanization time, etc., and achieves extended operation period, simple preparation process, The effect of broadening the reaction temperature range

Active Publication Date: 2014-05-21
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

[0028] (1) Preparation of impregnation solution

[0029] 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.

[0030] (2), loaded vulcanized active components

[0031] The palladium loading amount of the catalyst is designed to be 0.5wt%.

[0032] 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.

[0033] Measure 14 milliliters of impregnation solution containing palladium 0.15wt% in a 200 milliliter beaker, get 10g gamma-alumina (specific surface area 189m 2 / g, pore volume 0.4mL / g) was poured into it, dipped for 3 hours, then put the beaker in a water bath, heated at 65°C, and added dropwise 11ml of a solution containing 0.5wt% sodium ethyl xanthate, ethyl xanthate The molar ratio of sodium xanthate to palladium is 2.0:1, gently stirred...

Embodiment 2

[0037] (1) Same as embodiment 1

[0038] (2), loaded vulcanized active components

[0039] The palladium loading amount of the catalyst is designed to be 0.40wt%.

[0040] Put sodium propyl xanthate in a 200 ml beaker, add deionized water to dissolve, and prepare a solution containing 0.5wt% sodium propyl xanthate

[0041] Measure 10 milliliters of impregnating solution containing palladium 0.15wt% in a 200 milliliter beaker, pour 10 g of gamma-alumina (the same properties as in Example 1) into it, soak for 4 hours, then put the beaker into a water bath, heat at 70°C, Add dropwise 10 ml of a solution containing 0.5 wt% sodium propyl xanthate, the molar ratio of sodium propyl xanthate to palladium is 2.3:1, gently stir and impregnate for 4 hours, remove the residue by filtration, and dry at 115°C for 6 hours, the catalyst intermediate was obtained.

[0042] (3) Loaded oxidized active components

[0043] Measure 17 ml of impregnating solution containing 0.15 wt% palladium in...

Embodiment 3

[0045] (1) Same as embodiment 1

[0046] (2), loaded vulcanized active components

[0047] The palladium loading amount of the catalyst is designed to be 0.30wt%.

[0048] 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.

[0049] Measure 6 milliliters of the impregnating solution containing palladium 0.15 wt % in a 200 milliliter beaker, pour 10 g of γ-alumina (the same properties as in Example 1) into it, soak for 3 hours, then put the beaker into a water bath, and heat it at 65° C. Add dropwise 6 ml of a solution containing 0.5 wt% sodium ethyl xanthate, the molar ratio of sodium ethyl xanthate to palladium is 2.2:1, gently stir and impregnate for 4 hours, remove the residual liquid by filtration, and dry at 115°C for 6 hours, the catalyst intermediate was obtained.

[0050] (3) Loaded oxidized active components

[0051] Measure 14 ml of impregnation solution contai...

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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 impregnating solution containing palladium and impregnating an alumina carrier in a part of the impregnating solution containing palladium; then adding a proper amount of a sodium alkyl xanthate solution drop by drop, wherein a catalyst intermediate is obtained after impregnation; and impregnating the catalyst intermediate in the rest impregnating solution containing palladium and carrying out drying and roasting 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 a conventional oxidized palladium / alumina catalyst 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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IPC IPC(8): B01J37/20B01J23/44C07C49/04C07C45/73
Inventor 宋丽芝王海波勾连科薛冬
Owner CHINA PETROLEUM & CHEM CORP
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